Triethylamine → 4-iodo-N,N-dimethylbenzamide

HRID 230612노트

반응식

HRID 230612 반응식
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

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10473Dimethylamine, hydrochlorideHCID 743734-Iodobenzoyl chloride

생성물 1

HCID 8799334-iodo-N,N-dimethylbenzamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-254dea5b0d9a420fa7f12f1c1270b4a9
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07566735B2

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