Triphenylphosphine → HCID 86759695, 화합물

HRID 2179959

반응식

HRID 2179959 반응식
N(C(OCC)=O)=NC(OCC)=O.[CH3:13][C:14]([O:17][C:18](=[O:30])[NH:19][CH2:20][CH2:21][CH:22]([OH:29])[C:23]1[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=1)([CH3:16])[CH3:15].[Cl:31][C:32]1[CH:37]=[CH:36][C:35]([C:38]([F:41])([F:40])[F:39])=[CH:34][C:33]=1O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCCC1>[CH3:16][C:14]([O:17][C:18](=[O:30])[NH:19][CH2:20][CH2:21][CH:22]([O:29][C:33]1[CH:34]=[C:35]([C:38]([F:40])([F:41])[F:39])[CH:36]=[CH:37][C:32]=1[Cl:31])[C:23]1[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=1)([CH3:13])[CH3:15]

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 123498Phenol, 2-chloro-5-(trifluoromethyl)-HCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 69799429[3-Hydroxy-3-(3-pyridinyl)propyl]carbamic acid 1,1-dimethylethyl ester

생성물 1

HCID 86759695HCID 86759695, 화합물수율 79.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
20 °C

실험 절차

Diethyl azodicarboxylate (0.71 ml, 4.47 mmol) was added to a solution of [3-hydroxy-3-(3-pyridinyl)propyl]carbamic acid 1,1-dimethylethyl ester (Example 58(b)) (291 mg, 1.15 mmol), 2-chloro-5-trifluoromethylphenol (232 mg, 1.18 mmol) and triphenylphosphine (455 mg, 1.73 mmol) in tetrahydrofuran (6 ml) at 0° C. and stirred at 20° C. for 18 h. The reaction was concentrated in vacuo and the residue purified by chromatography on silica, eluting with petrol—diethyl ether to afford the sub-title compound (394 mg, 79%).

후처리

  1. concentrationThe reaction was concentrated in vacuo
  2. customthe residue purified by chromatography on silica
  3. washeluting with petrol—diethyl ether

출처 및 근거

ORD 기록
ord-01c5c48fb327480c8b357565e11d2b34
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06887871B2

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