Triethylamine → 4-iodo-N,N-dimethylbenzamide

HRID 230612ノート

反応式

HRID 230612 の反応式
Cl.[CH3:2][NH:3][CH3:4].C(N(CC)CC)C.[I:12][C:13]1[CH:21]=[CH:20][C:16]([C:17](Cl)=[O:18])=[CH:15][CH:14]=1>ClCCl>[I:12][C:13]1[CH:21]=[CH:20][C:16]([C:17]([N:3]([CH3:4])[CH3:2])=[O:18])=[CH:15][CH:14]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10473Dimethylamine, hydrochlorideHCID 743734-Iodobenzoyl chloride

生成物 1

HCID 8799334-iodo-N,N-dimethylbenzamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A suspension of dimethylamine hydrochloride (2.45 g, 30 mmol) in dichloromethane (150 ml) was cooled in an ice/methanol bath and then treated with triethylamine (6.0 g, 59 mmol) followed by 4-iodobenzoyl chloride (8.0 g, 30 mmol) portionwise with stirring under an atmosphere of argon. The reaction mixture was allowed to stir at room temperature for 30 minutes before the solution was washed with water (2×100 ml). The organic layer was separated, dried over sodium sulphate, and evaporated under reduced pressure to give the title compound as a light beige coloured solid (7.73 g, 94%).

後処理

  1. temperaturewas cooled in an ice/methanol bath
  2. stirringto stir at room temperature for 30 minutes before the solution
  3. washwas washed with water (2×100 ml)
  4. customThe organic layer was separated
  5. dry with materialdried over sodium sulphate
  6. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-254dea5b0d9a420fa7f12f1c1270b4a9
出典データセット
uspto-grants-2009_07
特許番号
US07566735B2

反応ノート

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