Lithium Hydroxide → N-Boc-N-methylethylenediamine

HRID 2234673노트

반응식

HRID 2234673 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 2756424N-Boc-N-methylethylenediamine수율 18%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-ce4f9f51668a4670861bb07c2cda3835
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709645B2

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