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

HRID 730833笔记

反应方程式

HRID 730833 反应方程式
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]

参与物

4

反应物 2

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

产物 1

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

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

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).

后处理

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

来源与证据

ORD记录
ord-4c5de376c51f4c09b22f26f2de526a00
来源数据集
uspto-grants-2009_09
专利号
US07582761B2

反应笔记

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