Triethylamine → N'-(cyclopropanecarbonyl)-3-iodo-4-methylbenzohydrazide

HRID 1619147

反応式

HRID 1619147 の反応式
[CH:1]1([C:4](Cl)=[O:5])[CH2:3][CH2:2]1.[I:7][C:8]1[CH:9]=[C:10]([CH:15]=[CH:16][C:17]=1[CH3:18])[C:11]([NH:13][NH2:14])=[O:12].C(N(CC)CC)C>ClCCl>[CH:1]1([C:4]([NH:14][NH:13][C:11](=[O:12])[C:10]2[CH:15]=[CH:16][C:17]([CH3:18])=[C:8]([I:7])[CH:9]=2)=[O:5])[CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 77637Cyclopropanecarbonyl chlorideHCID 597325003-Iodo-4-methylbenzohydrazide

生成物 1

HCID 965865N'-(cyclopropanecarbonyl)-3-iodo-4-methylbenzohydrazide収率 76.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of cyclopropanecarbonyl chloride (1.81 mL, 20.0 mmol) in dichloromethane (20 mL) was added dropwise to a stirred solution of 3-iodo-4-methylbenzohydrazide (preparation 55b, 5.00 g, 18.1 mmol) and triethylamine (2.78 mL, 20.0 mmol) in dichloromethane (80 mL) at 0° C. After 2 hours stirring at ambient temperature, the mixture was concentrated in vacuo and water was added to the residue. The resultant precipitate was filtered and was washed with water and diethyl ether to give the title compound (4.75 g, 76%) as a white solid.

後処理

  1. concentrationthe mixture was concentrated in vacuo and water
  2. additionwas added to the residue
  3. filtrationThe resultant precipitate was filtered
  4. washwas washed with water and diethyl ether

出典と根拠

ORDレコード
ord-858db07679aa403c948126bf8853f46d
出典データセット
uspto-grants-2014_07
特許番号
US08772288B2

関連ノート

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