Triphenylphosphine → HCID 86651838、化合物

HRID 1465446ノート

反応式

HRID 1465446 の反応式
[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]

参加物

4

反応物 2

HCID 11776TriphenylphosphineHCID 67266620HCID 67266620、化合物

生成物 1

HCID 86651838HCID 86651838、化合物収率 78.5%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d805eba4b89d4119a13c71d88d8163c5
出典データセット
uspto-grants-2015_04
特許番号
US08999989B2

反応ノート

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