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Tert-Butylamine → HCID 25239132, 화합물

HRID 555989
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HRID 555989 반응식
[NH:1]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:2][CH2:3][C:4]([OH:6])=O.[C:14]([NH2:18])([CH3:17])([CH3:16])[CH3:15]>C(Cl)Cl>[C:10]([O:9][C:7](=[O:8])[NH:1][CH2:2][CH2:3][C:4](=[O:6])[NH:18][C:14]([CH3:17])([CH3:16])[CH3:15])([CH3:13])([CH3:12])[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6385Tert-ButylamineHCID 76809N-((1,1-dimethylethoxy)carbonyl)-beta-alanine

생성물 1

HCID 25239132HCID 25239132, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

BOC-Beta-Ala-OH (25 g, 0.132 mol) is dissolved in DCM (500 ml) and then treated with EDC1 (30.4 g, 0.59 mol) followed by t-butylamine (16.7 ml, 0.159 mol) to give a pale orange solution. The reaction mixture is stirred at room temperature overnight and then partitioned between 20% citric acid (400 ml) and DCM (250 ml). The organic portion is separated and washed with water (400 ml), saturated NaHCO3 (400 ml), brine (400 ml), dried over MgSO4 and concentrated in vacuo to afford the title compound as a white solid.

후처리

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  1. additiontreated with EDC1 (30.4 g, 0.59 mol)
  2. customto give a pale orange solution
  3. custompartitioned between 20% citric acid (400 ml) and DCM (250 ml)
  4. customThe organic portion is separated
  5. washwashed with water (400 ml), saturated NaHCO3 (400 ml), brine (400 ml)
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-1bb55408e5d34ace87849c8b3aa1ea81
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08053574B2

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