Triphenylphosphine → Methyl 3-(4-{{[4'-(2-ethoxyethoxy)-2',6'-dimethylbiphenyl-3-yl]methyl}[(2-nitrophenyl)sulfonyl]amino}phenyl)propanoate

HRID 508030ノート

反応式

HRID 508030 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10]([NH:13][C:14]1[CH:19]=[CH:18][C:17]([CH2:20][CH2:21][C:22]([O:24][CH3:25])=[O:23])=[CH:16][CH:15]=1)(=[O:12])=[O:11])([O-:3])=[O:2].[CH2:26]([O:28][CH2:29][CH2:30][O:31][C:32]1[CH:37]=[C:36]([CH3:38])[C:35]([C:39]2[CH:44]=[CH:43][CH:42]=[C:41]([CH2:45]O)[CH:40]=2)=[C:34]([CH3:47])[CH:33]=1)[CH3:27].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>C1(C)C=CC=CC=1>[CH2:26]([O:28][CH2:29][CH2:30][O:31][C:32]1[CH:37]=[C:36]([CH3:38])[C:35]([C:39]2[CH:44]=[CH:43][CH:42]=[C:41]([CH2:45][N:13]([S:10]([C:5]3[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=3[N+:1]([O-:3])=[O:2])(=[O:12])=[O:11])[C:14]3[CH:19]=[CH:18][C:17]([CH2:20][CH2:21][C:22]([O:24][CH3:25])=[O:23])=[CH:16][CH:15]=3)[CH:40]=2)=[C:34]([CH3:47])[CH:33]=1)[CH3:27]

参加物

6

反応物 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 23111752[4'-(2-Ethoxyethoxy)-2',6'-dimethylbiphenyl-3-yl]methanolHCID 23157467Methyl 3-(4-{[(2-nitrophenyl)sulfonyl]amino}phenyl)propanoate

生成物 1

HCID 23157381Methyl 3-(4-{{[4'-(2-ethoxyethoxy)-2',6'-dimethylbiphenyl-3-yl]methyl}[(2-nitrophenyl)sulfonyl]amino}phenyl)propanoate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of methyl 3-(4-{[(2-nitrophenyl)sulfonyl]amino}phenyl)propanoate (0.802 g, 2.20 mmol), [4′-(2-ethoxyethoxy)-2′,6′-dimethylbiphenyl-3-yl]methanol (0.601 g, 2.00 mmol) and triphenylphosphine (1.05 g, 4.00 mmol) in toluene (40 mL) was stirred under ice-cooling, and diethyl azodicarboxylate (40% toluene solution, 1.81 mL, 4.00 mmol) was added. The mixture was allowed to warm to room temperature and stirred for 43 hr. The reaction mixture was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (20%-60% ethyl acetate/hexane) to give the title compound as an orange oil.

後処理

  1. temperaturecooling
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customthe residue was purified by silica gel column chromatography (20%-60% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-63d89aa545bf4a18b497bd5ae08ef786
出典データセット
uspto-grants-2010_08
特許番号
US07786165B2

反応ノート

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