Acetyl chloride → HCID 22668555、化合物

HRID 1883729ノート

反応式

HRID 1883729 の反応式
[CH3:1][N:2]([CH3:15])[CH2:3][CH2:4][NH:5][C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[CH:8][CH:7]=1.C(N(CC)CC)C.[C:23](Cl)(=[O:25])[CH3:24]>C(Cl)Cl>[CH3:1][N:2]([CH3:15])[CH2:3][CH2:4][N:5]([C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[CH:8][CH:7]=1)[C:23](=[O:25])[CH3:24]

参加物

5

反応物 3

HCID 6367Acetyl chloride2 回HCID 8471Triethylamine2 回HCID 22569398HCID 22569398、化合物

生成物 1

HCID 22668555HCID 22668555、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3.6 g of 4-(2-dimethylamino-ethylamino)-nitrobenzene (according to Gabbay et al., J. Am. Chem. Soc. 91, 5136 (1969)) are dissolved in 50 ml of methylene chloride and 5.0 ml of triethylamine are added. 1.3 ml of acetyl chloride are slowly added dropwise to this mixture at room temperature and the mixture is stirred for 2 hours at room temperature. After this time another 5.0 ml of triethylamine and 1.3 ml of acetylchloride are added and the mixture is refluxed for another 2 hours. The solvent is removed, the residue is taken up in ethyl acetate and the organic phase is extracted twice with water. After drying over MgSO4 the solvent is removed and the residue dried in vacuo.

後処理

  1. temperaturethe mixture is refluxed for another 2 hours
  2. customThe solvent is removed
  3. extractionthe organic phase is extracted twice with water
  4. dry with materialAfter drying over MgSO4 the solvent
  5. customis removed
  6. customthe residue dried in vacuo

出典と根拠

ORDレコード
ord-43b54c6d082b4b848d95077a75a21096
出典データセット
uspto-grants-2004_07
特許番号
US06762180B1

反応ノート

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