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

HRID 730833ノート

反応式

HRID 730833 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-4c5de376c51f4c09b22f26f2de526a00
出典データセット
uspto-grants-2009_09
特許番号
US07582761B2

反応ノート

読み込み中…