4-Benzyloxycarbonylamino-4-hydroxymethyl piperidine-1-carboxylic acid tert-butyl ester → tert-Butyl 4-amino-4-(hydroxymethyl)piperidine-1-carboxylate

HRID 2193072ノート

反応式

HRID 2193072 の反応式
C(OC([NH:11][C:12]1([CH2:25][OH:26])[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:14][CH2:13]1)=O)C1C=CC=CC=1>[OH-].[Pd+2].[OH-].[C].C(O)C>[NH2:11][C:12]1([CH2:25][OH:26])[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:22])([CH3:23])[CH3:24])=[O:19])[CH2:14][CH2:13]1

参加物

4

反応物 1

HCID 667417704-Benzyloxycarbonylamino-4-hydroxymethyl piperidine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 22975819tert-Butyl 4-amino-4-(hydroxymethyl)piperidine-1-carboxylate

試薬・触媒・溶媒 2

HCID 178502593HCID 178502593、化合物触媒HCID 702Ethanol溶媒

反応条件

温度
40 °C

実験手順

To 10 mL of an ethanol solution containing 0.55 g of tert-butyl 4-(((benzyloxy)carbonyl)amino)-4-(hydroxymethyl)piperidine-1-carboxylate, 0.10 g of 20% palladium hydroxide-carbon was added at room temperature, and the mixture was stirred at 40° C. for 3 hours under a hydrogen atmosphere. The insoluble material filtered off, and the filtration residue thus obtained was washed 3 times with chloroform. The filtrate and the washing solution were combined, and the solvent was removed under reduced pressure to obtain 0.39 g of a dark brown oily substance, tert-butyl 4-amino-4-(hydroxymethyl)piperidine-1-carboxylate.

後処理

  1. additionwas added at room temperature
  2. filtrationThe insoluble material filtered off
  3. customthe filtration residue thus obtained
  4. washwas washed 3 times with chloroform
  5. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-9659172582a24218b9bc40bf467ea604
出典データセット
uspto-grants-2012_12
特許番号
US08329694B2

反応ノート

読み込み中…