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Purification of Organic Chemicals 24 1
N-Hydroxy-5-norbornene-2,3-dicarboxylic acid imide [21715-90-21 M 179.2, m 165-166O,
166-169O Dissolve in CHC13, filter, evaporate and recrystallise from EtOAc. IR (nujol): 1695, 1710 and
1770 (C=O), and 3100 (OH) cm-I. 0-Acefyl derivative has m 113-1 14O (from EtOH) with IR bands at 1730,
1770 and 1815 cm-I only, and the 0-benzoyl derivative has m 143-144O (from propan-2-01 or C6H6). [Bauer
and Miarka JOC 24 1293 1959; Fujino et al. Chem Pharm Bull Japan 22 1857 19741.
DL-erythro-3-Hydroxynorvaline (2-amino-3-hydroxypentanoic acid) [34042-00-71 M 133.2,
m 257-259O (dec), 263O (dec). Purified by recrystn from aqueous EtOH. The Cu salt has m 255-256O
(dec), the benzoyl derivative has rn 181°, and the N-phenylcarbamoyl derivative has m 164O. [Buston et al.
JBC 204 665 19531.
2-Hydroxyoctanoic acid [617-73-21 M 160.2, m 69.5O. Crystd from EtOH/pet ether or
ether/ligroin.
1-Hydroxyphenazine [528-71-21 M 196.2, m 157-158O. Chromatographed on acidic alumina with
benzene/ether. Crystd from benzeneheptane, and sublimed.
2-Hydroxyphenylacetic acid [614-75-51 M 152.2, m 148-149O, b 240-243°/760mrn. Crystd
from ether or chloroform.
3-Hydroxyphenylacetic acid [621-37-41 M 152.2, rn 137O. Crystd from benzene/ligroin.
4-Hydroxyphenylacetic acid [156-38-71 M 152.2, m 150-15lo. Crystd from water.
2-(2-Hydroxyphenyl)benzothiazole [341 I-95-81 M 227.2, m 132-133O, b 173-179O/3 mm.
2-(2-Hydroxyphenyl)benzoxazole [835-64-31 M 211.2, m 127O, b 33S0/760rnm,
Recrystd several times from aqueous EtOH and by sublimation. [Itoh and Fujiwara JACS 107 1561 19851.
3-Hydroxy-2-phenylcinchoninic acid [485-89-21 M 265.3, m 206-207O(dec). Crystd from
EtOH.
N-(p-Hydroxypheny1)glycine [122-87-21 M 167.2, m >240°(dec). Crystd from water.
N- (4-Hydroxyphenyl)-3-phenylsalicylarnide [550-57-21 M 305.3, rn 183-184O. Crystd from
aqueous MeOH.
L-2-Hydroxy-3-phenylpropionic acid (phenyl lactic acid) [20312-36-11 M 166.2, rn 125-
126O, [0r]i2 -18.7O (EtOH). Crystd from water, MeOH, EtOH or benzene.
dl-2-Hydroxy-3-phenylpropionic acid [828-01-31 M 166.2, m 97-9S0, b 148-150°/ 15 m rn.
Crystd from benzene or chloroform.
3-Hydroxy-2-phenylpropionic acid see tropic acid.
3-p-Hydroxyphenylpropionic acid [Sol -97-31 M 166.2, rn 129-130°. Crystd from ether.
p-Hydroxyphenylpyruvic acid [156-39-81 M 180.2, m 220O. Crystd three times from 0.1M
HClEtOH (4: 1, v/v) immediately before use [Rose and Powell BJ 87 541 19631.
N-Hydroxyphthalimide [524-38-91 M 163.1, m 230°, -235O (dec), 237-240°. Dissolve in H20
by adding Et,N to form the salt and while hot acidify, cool and pour into a large volume of H20. Filter off the
solid, wash with H20, dry over P2O5 in vacuum. [Nefken And Teser JACS 83 1263 1961; Fieser 1 485 1976;
Nefkens et al. Rec Truv Chim Pays Bus 81 683 19621 The 0-aceryl derivative has m 178-180° (from
EtOH).