Dichloromethane piperidine → (3R)-3-Butyl-2,5-piperazinedione

HRID 730833노트

반응식

HRID 730833 반응식
C1C2C(COC([NH:18][C@@H:19]([C:24]([NH:26][CH2:27][C:28]([O:30]C)=O)=[O:25])[CH2:20][CH2:21][CH2:22][CH3:23])=O)C3C(=CC=CC=3)C=2C=CC=1.ClCCl.N1CCCCC1>ClCCl>[CH2:20]([C@H:19]1[NH:18][C:28](=[O:30])[CH2:27][NH:26][C:24]1=[O:25])[CH2:21][CH2:22][CH3:23]

참가 물질

4

반응물 2

HCID 67144590Dichloromethane piperidineHCID 67401200Methyl N-{[(9H-fluoren-9-ylmethyl)oxy]carbonyl}-D-norleucylglycinate

생성물 1

HCID 67400830(3R)-3-Butyl-2,5-piperazinedione

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of methyl N-{[(9H-fluoren-9-ylmethyl)oxy]carbonyl}-D-norleucylglycinate from step (a) above (2 g, 4.7 mmol) in a 7:3 mixture of dichloromethane/piperidine (30 mL) was stirred at room temperature for 0.75 h. The reaction mixture was diluted with dichloromethane (200 mL) and solid which precipitated was filtered, washed with cold DCM (2×50 mL) and dried in vacuo to give the title compound as a white solid. MS (ESI, positive ion) m/z: 171 (M+1).

후처리

  1. customprecipitated
  2. filtrationwas filtered
  3. washwashed with cold DCM (2×50 mL)
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-4c5de376c51f4c09b22f26f2de526a00
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07582761B2

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