Synthese und Eigenschaften hydrophiler Arylphosphane

10 Experimenteller Teil 111
Nr. g (mmol)
Jodaromat
17 7.84 (26.9)
5-Jodisophthalsäure
4
18 7.06 (26.85)
5-Jodanthranilsäure
19 13.2 (50)
3-Hydroxy-4jod-benzoesäure
20 71.32
(5)
4-Hydroxy-3jod-benzoesäure
21 69.85
(37.6)
3-Jod-4-methylbenzoesäure
97%
22 8.76 (30)
4-Jodphthalsäure
5
25 27.8 (100)
3-Jod-5-methylsalicylsäure
1
26 11.6 (37.6)
4-Hydroxy-5jodi
h h l 2
Tab. 4 (Fortsetzung)
g Ph2PH
(mmol)
5.0
(26.9)
5.0
(26.85)
9.31
(50)
0.93
(5)
7.0
(37.6)
5.59
(30)
18.6
(100)
7.0
(36.7)
CH3CN
ml
Pd(OAc)2
mg(μmol)
g NEt3
(mmol)
60 3.0 (13) 8.15
(81)
60 6.0
(26.7)
5.46
(54)
100 5.6 (25) 10.2
(100)
10 1.1 (5) 1.02
(10)
90 8.5 (38) 8.1
(80)
80 6.7 (30) 9.1
(90)
250 22.5
(100)
90 8.5
(38)
20.2
(200)
12.1
(120)
Reaktionsbedingungen
12 h /
85°C
50 h /
85°C
18 h /
100°C
KOH
1N
(ml)
Umkrist.
aus
85 Ethanol /
Wasser
Ausbeute
g (%)
7.25
(77)
60 - 8.1
(94)
100 CH2Cl2 10.6
(66)
48 h / 90 10 CH2Cl2 0.79
(49)
18 h /
90°C
48 h /
100°C
48 h /
90°C
40 h /
85°C
80 CH2Cl2 7.32
(61)
90 Ethanol /
Wasser
8.41
(80)
220 CH2Cl2 22.2
(67)
120 Ethanol /
Wasser
9.39
(68)
Summenformel
Elementaranalyse
ber. Elementaranalyse
C20H15O4P
EA : 67.43%C, 5.32%H
ber.: 68.57%C, 4.32%H
C19H16NO2P
EA : 70.65%C, 5.49%H, 4.11%N
ber.: 71.02%C, 5.02%H, 4.36%N
C19H15O3P
EA : 68.68%C, 4.96%H
ber.: 70.81%C, 4.69%H
C19H15O3P
EA : 69.34%C, 4.84%H
ber.: 70.81%C, 4.69%H
C20H17O2P
EA : 74.63%C, 5.50%H
ber.: 74.99%C, 5.35%H
C20H15O4P
EA : 69.60%C, 5.05%H
ber.: 68.57%C, 4.32%H
C20H17O3P
EA : 69.73%C, 5.33%H
ber.: 71.42%C, 5.09%H
C20H15O5P
EA : 64.92%C, 4.37%H
ber.: 65.58%C, 4.13%H