HCID 86701036、化合物 → 1,1-Dimethylethyl N-[1-(2-hydroxyethyl)cyclopropyl]carbamate

HRID 1427659ノート

反応式

HRID 1427659 の反応式
[Si]([O:8][CH2:9][CH2:10][C:11]1([NH:14][C:15](=[O:21])[O:16][C:17]([CH3:20])([CH3:19])[CH3:18])[CH2:13][CH2:12]1)(C(C)(C)C)(C)C>C(Cl)Cl>[OH:8][CH2:9][CH2:10][C:11]1([NH:14][C:15](=[O:21])[O:16][C:17]([CH3:19])([CH3:18])[CH3:20])[CH2:12][CH2:13]1

参加物

3

反応物 1

HCID 86701036HCID 86701036、化合物

生成物 1

HCID 129931391,1-Dimethylethyl N-[1-(2-hydroxyethyl)cyclopropyl]carbamate収率 60.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of tert-butyl 1-(2-(tert-butyldimethylsilyloxy)ethyl)cyclopropylcarbamate (11.9 g, 37.8 mmol) and 3HF.TEA (22.0 g) in DCM (50 mL) was stirred at rt for 17 hrs. The mixture was concentrated and the residue was purified by silica gel column chromatography (0˜20% gradient elution EtOAc/petroleum ether) to afford tert-butyl 1-(2-hydroxyethyl)cyclopropylcarbamate (4.6 g, 60%) as a white solid.

後処理

  1. concentrationThe mixture was concentrated
  2. customthe residue was purified by silica gel column chromatography (0˜20% gradient elution EtOAc/petroleum ether)

出典と根拠

ORDレコード
ord-4df83041561b4c7a9628c825ba8285b9
出典データセット
uspto-grants-2015_01
特許番号
US08933233B2

反応ノート

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