Water → Fla 908

HRID 414076

반응식

HRID 414076 반응식
Cl.[CH2:2]([N:4]1[CH2:8][CH2:7][CH2:6][CH:5]1[CH2:9][NH:10][C:11](=[O:22])[C:12]1[C:17]([O:18]C)=[CH:16][CH:15]=[CH:14][C:13]=1[O:20][CH3:21])[CH3:3].B(Br)(Br)[Br:24].O>ClCCl>[CH2:2]([N:4]1[CH2:8][CH2:7][CH2:6][CH:5]1[CH2:9][NH:10][C:11](=[O:22])[C:12]1[C:17]([OH:18])=[CH:16][CH:15]=[C:14]([Br:24])[C:13]=1[O:20][CH3:21])[CH3:3]

참가 물질

5

반응물 3

HCID 962WaterHCID 25134Boron tribromideHCID 15565705N-ethyl-2-(2,6-dimethoxybenzamidomethyl)pyrrolidine hydrochloride

생성물 1

HCID 129516Fla 908수율 80%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of N-ethyl-2-(2,6-dimethoxybenzamidomethyl)pyrrolidine hydrochloride (23.0 g, 0.07 mole) in 300 ml of dry dichloromethane was added dropwise with stirring a solution of boron tribromide (17.5 g, 0.07 mole) in 25 ml of dry dichloromethane at 0° C. After the addition was completed the solution was allowed to reach room temperature over night. Water was added and pH adjusted to 7. The organic layer was washed with water and dried (MgSO4). The solvent was evaporated in vacuo affording the title compound as a viscous oil (20 g) which was judged by TLC and GC analysis to be sufficiently pure for use in the next step without further purification.

후처리

  1. additionAfter the addition
  2. waitto reach room temperature over night
  3. washThe organic layer was washed with water
  4. dry with materialdried (MgSO4)
  5. customThe solvent was evaporated in vacuo

출처 및 근거

ORD 기록
ord-14f236f8f86b4156bdd47a43d0de1895
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04789683

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