Acetic Anhydride → N-[2-(tert-Butoxycarbonylmethylamino)ethyl]-N-methylacetamide

HRID 17494ノート

反応式

HRID 17494 の反応式
C(OC(=O)C)(=[O:3])C.[CH2:8]([N:10]([CH2:13][CH3:14])[CH2:11][CH3:12])C.[C:15]([O:19][C:20]([CH2:22][NH:23]CCNC)=[O:21])([CH3:18])([CH3:17])[CH3:16]>ClCCl>[C:15]([O:19][C:20]([CH2:22][NH:23][CH2:12][CH2:11][N:10]([CH3:8])[C:13](=[O:3])[CH3:14])=[O:21])([CH3:18])([CH3:17])[CH3:16]

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 59921864HCID 59921864、化合物

生成物 1

HCID 86630858N-[2-(tert-Butoxycarbonylmethylamino)ethyl]-N-methylacetamide収率 100%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Under nitrogen atmosphere, acetic anhydride (1.16 ml, 12.3 mmol) and triethylamine (2.28 ml, 16.4 mmol) were added to a dichloromethane (41 ml) solution of [2-(tert-butoxycarbonylmethylamino)ethyl]methylamine (I-202) (1.54 g, 8.18 mmol) with cooling with ice, followed by stirring at room temperature for 15 hours. The solvent was evaporated away under reduced pressure, then the resulting residue was subjected to silica gel column chromatography, and the eluate with dichloromethane/methanol (10:1, v/v) gave the entitled compound (1.88 g, 100%) as a colorless oil.

後処理

  1. temperaturewith cooling with ice
  2. customThe solvent was evaporated away under reduced pressure

出典と根拠

ORDレコード
ord-422600918c5448baa5b1af786fee5d8d
出典データセット
uspto-grants-2010_06
特許番号
US07737166B2

反応ノート

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