Methylamine → tert-Butyl 3-(methylamino)pyrrolidine-1-carboxylate

HRID 888952ノート

反応式

HRID 888952 の反応式
[C:1]([N:8]1[CH2:12][CH2:11][C:10](=O)[CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[CH3:14][NH2:15].[BH4-].[Na+]>CO.ClCCl>[C:4]([O:3][C:1]([N:8]1[CH2:12][CH2:11][CH:10]([NH:15][CH3:14])[CH2:9]1)=[O:2])([CH3:7])([CH3:6])[CH3:5]

参加物

6

反応物 3

HCID 6329MethylamineHCID 471360Tert-butyl 3-oxopyrrolidine-1-carboxylateHCID 4311764Sodium borohydride

生成物 1

HCID 45089533tert-Butyl 3-(methylamino)pyrrolidine-1-carboxylate収率 98%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1-N-BOC-3-pyrrolidinone (3.0 g) in methanol (30 ml) was added a solution of freshly prepared methylamine (0.75 g) in methanol (3.1 ml). The reaction mixture was stirred for 1 hour and then sodium borohydride (0.61 g) was added. After stirring for 4 hours the reaction mixture was then diluted with dichloromethane, washed with sodium bicarbonate solution, dried (MgSO4) and the solvent removed in vacuo to give 3-methylamino-pyrrolidine-1-carboxylic acid tert-butyl ester (3.18 g).

後処理

  1. stirringAfter stirring for 4 hours the reaction mixture
  2. washwashed with sodium bicarbonate solution
  3. dry with materialdried (MgSO4)
  4. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-149d3e184f4c4809bd98e58b8bb7c516
出典データセット
uspto-grants-2012_08
特許番号
US08252792B2

反応ノート

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