Lithium Hydroxide → N-Boc-N-methylethylenediamine

HRID 2234673ノート

反応式

HRID 2234673 の反応式
[C:1]([O:5][C:6](=[O:18])[N:7]([CH3:17])[CH2:8][CH2:9][NH:10]C(=O)C(F)(F)F)([CH3:4])([CH3:3])[CH3:2].[OH-].[Li+]>CO>[C:1]([O:5][C:6](=[O:18])[N:7]([CH2:8][CH2:9][NH2:10])[CH3:17])([CH3:4])([CH3:2])[CH3:3]

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 10635722Methyl-[2-(2,2,2-trifluoro-acetylamino)-ethyl]-carbamic acid tert-butyl ester

生成物 1

HCID 2756424N-Boc-N-methylethylenediamine収率 18%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of methyl-[2-(2,2,2-trifluoro-acetylamino)-ethyl]-carbamic acid tert-butyl ester (1.04 g, 3.85 mmol) in methanol (60 mL) was added 1 M aqueous lithium hydroxide (34 mL, 34.00 mmol). The mixture was stirred at room temperature overnight. It was then concentrated and ethyl acetate (50 mL) was added. The precipitate was filtered off and the filtrate concentrated to give 120 mg (18%) of (2-amino-ethyl)-methyl-carbamic acid tert-butyl ester. 1H-NMR (250 MHz, CDCl3) δ 3.22 (t, J=6.5 Hz, 2H), 2.72-2.86 (m, 5H), 1.36 (s, 9H).

後処理

  1. concentrationIt was then concentrated
  2. additionethyl acetate (50 mL) was added
  3. filtrationThe precipitate was filtered off
  4. concentrationthe filtrate concentrated

出典と根拠

ORDレコード
ord-ce4f9f51668a4670861bb07c2cda3835
出典データセット
uspto-grants-2010_05
特許番号
US07709645B2

反応ノート

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