Water → Fla 908

HRID 414076ノート

反応式

HRID 414076 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 129516Fla 908収率 80%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-14f236f8f86b4156bdd47a43d0de1895
出典データセット
uspto-grants-1988_12
特許番号
US04789683

反応ノート

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