Triethylamine → N-(3-chloropropyl)-4-nitrobenzamide

HRID 1601338

反応式

HRID 1601338 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][NH2:5].C(N(CC)CC)C.[N+:13]([C:16]1[CH:24]=[CH:23][C:19]([C:20](Cl)=[O:21])=[CH:18][CH:17]=1)([O-:15])=[O:14]>C(Cl)Cl>[Cl:1][CH2:2][CH2:3][CH2:4][NH:5][C:20](=[O:21])[C:19]1[CH:18]=[CH:17][C:16]([N+:13]([O-:15])=[O:14])=[CH:24][CH:23]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 85024-Nitrobenzoyl chlorideHCID 846293-Chloropropylamine

生成物 1

HCID 3421653N-(3-chloropropyl)-4-nitrobenzamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 6.43 g (49 mmol) 3-chloropropylamine and 13.6 ml (98 mmol) triethylamine in 220 ml methylene chloride was cooled by an ice bath and 9 g (48.5 mmol) 4-nitrobenzoyl chloride were added fractionwise. After one hour stirring at room temperature the organic phase was washed twice with water, dried over MgSO4 and concentrated in vacuo to afford 10.68 g (91%). of beige crystals. 1H NMR was consistent with the desired structure.

後処理

  1. washwas washed twice with water
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated in vacuo
  4. customto afford 10.68 g (91%)

出典と根拠

ORDレコード
ord-f96156a5394c4311839ffe582a66b357
出典データセット
uspto-grants-1999_11
特許番号
US05977179

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