Triphenylphosphine → HCID 86651838, 화합물

HRID 1465446노트

반응식

HRID 1465446 반응식
[Cl:1][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]([NH:12][NH:13][C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])=[O:11])=[CH:5][CH:4]=1.[C:21]1([P:27]([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>C1C=CC=CC=1>[Cl-:1].[C:17]([O:16][C:14]([NH:13][NH:12][C:10]([CH2:9][C:6]1[CH:7]=[CH:8][C:3]([CH2:2][P+:27]([C:28]2[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=2)([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)=[CH:4][CH:5]=1)=[O:11])=[O:15])([CH3:20])([CH3:19])[CH3:18]

참가 물질

4

반응물 2

HCID 11776TriphenylphosphineHCID 67266620HCID 67266620, 화합물

생성물 1

HCID 86651838HCID 86651838, 화합물수율 78.5%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A mixture of tert-butyl 2-{[4-(chloromethyl)phenyl]acetyl}hydrazinecarboxylate (5.9 g, 19.7 mmol), triphenylphosphine (5.18 g, 19.7 mmol) and benzene (15 ml) was heated under reflux for 21 hrs. After cooling to room temperature, the precipitate was collected by filtration, washed 3 times with benzene, and dried under reduced pressure to give {4-[2-(tert-butoxycarbonyl)hydrazinocarbonylmethyl]benzyl}(triphenyl)phosphonium chloride (8.68 g, yield 78%) as a white solid.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 21 hrs
  3. filtrationthe precipitate was collected by filtration
  4. washwashed 3 times with benzene
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-d805eba4b89d4119a13c71d88d8163c5
출처 데이터셋
uspto-grants-2015_04
특허 번호
US08999989B2

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