Dichloromethane → HCID 68428933、化合物

HRID 2240287ノート

反応式

HRID 2240287 の反応式
ClCCl.[CH3:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([NH:12][NH2:13])=[CH:8][CH:7]=1.C(N(CC)CC)C.[C:21](Cl)(=[O:26])[C:22]([CH3:25])([CH3:24])[CH3:23]>O>[CH3:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([NH:12][NH:13][C:21](=[O:26])[C:22]([CH3:25])([CH3:24])[CH3:23])=[CH:8][CH:7]=1

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 62493Pivaloyl chlorideHCID 77023(4-Methoxyphenyl)hydrazine

生成物 1

HCID 68428933HCID 68428933、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a mixture of 50 ml of dichloromethane and 2.76 g of free 4-methoxyphenyl-hydrazine there are added first 2.2 g of triethylamine and then, dropwise, at a temperature of from 0° to 5°, 2.65 g of pivaloyl chloride. The reaction mixture is stirred for 12 hours at room temperature and then discharged into water. The aqueous mixture is extracted with dichloromethane, the extract is concentrated and the residue is recrystallised from toluene/pentane, yielding N-(4-methoxyphenyl)-N′-pivaloyl-hydrazine which melts at from 126° to 127°.

後処理

  1. extractionThe aqueous mixture is extracted with dichloromethane
  2. concentrationthe extract is concentrated
  3. customthe residue is recrystallised from toluene/pentane

出典と根拠

ORDレコード
ord-2fabd1ebcf9a44c6b47c6be027082d0f
出典データセット
uspto-grants-2010_05
特許番号
US07723362B2

反応ノート

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