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

HRID 508030노트

반응식

HRID 508030 반응식
[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]

참가 물질

6

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-63d89aa545bf4a18b497bd5ae08ef786
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07786165B2

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