Phosgene → (3S)-oxolan-3-yl carbonochloridate

HRID 263790

반응식

HRID 263790 반응식
[C:1]([Cl:4])(Cl)=[O:2].[OH:5][C@H:6]1[CH2:10][CH2:9][O:8][CH2:7]1>C1(C)C=CC=CC=1>[O:8]1[CH2:9][CH2:10][C@H:6]([O:5][C:1]([Cl:4])=[O:2])[CH2:7]1

참가 물질

4

반응물 2

HCID 6371Phosgene2회HCID 2733227(S)-(+)-3-Hydroxytetrahydrofuran

생성물 1

HCID 22876378(3S)-oxolan-3-yl carbonochloridate

시약·촉매·용매 1

HCID 1140Toluene용매3회

실험 절차

14.1 ml (27.24 mmol) of a 20% solution of phosgene in toluene are added dropwise to 14 ml of toluene. After the mixture has been cooled in an ice-bath, a solution of 2 g (22.7 mmol) of (S)-(+)3-hydroxy-tetrahydrofuran (JPS CHIMIE, Bevaix, Switzerland) in a small amount of toluene is added, the mixture is then stirred for 1 h at RT, and the excess phosgene is expelled with argon. After concentration in a rotary evaporator at reduced pressure, distillation is carried out for the purpose of purification. Boiling point at 12 torr: 130° C.

후처리

  1. temperatureAfter the mixture has been cooled in an ice-bath
  2. concentrationAfter concentration
  3. customin a rotary evaporator
  4. distillationat reduced pressure, distillation
  5. customis carried out for the purpose of purification
  6. custom130° C.

출처 및 근거

ORD 기록
ord-585b6fd97ddb4c2183512766e8014f98
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05643878

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