N,N-Dimethylaniline → Cyclopentylmethyl carbonochloridate

HRID 851712노트

반응식

HRID 851712 반응식
CN(C)C1C=CC=CC=1.[CH:10]1([CH2:15][OH:16])[CH2:14][CH2:13][CH2:12][CH2:11]1.[C:17](Cl)([Cl:19])=[O:18].C1(C)C=CC=CC=1>>[Cl:19][C:17]([O:16][CH2:15][CH:10]1[CH2:14][CH2:13][CH2:12][CH2:11]1)=[O:18]

참가 물질

5

반응물 4

HCID 949N,N-DimethylanilineHCID 1140TolueneHCID 6371PhosgeneHCID 77195Cyclopentanemethanol

생성물 1

HCID 13077898Cyclopentylmethyl carbonochloridate수율 81%

실험 절차

A mixture of 24.2 g (0.20 mole) N,N-dimethylaniline and 20.3 g (0.20 mole) of cyclopentylmethanol was slowly added to a 20% solution of phosgene in toluene (104 ml, 0.20 mole) cooled to -5° to +5° C. After the addition the reaction mixture was allowed to attain room temperature and was kept at room temperature for 30 min. The precipitate was filtered off and the solvent was evaporated. Distillation in vacuo gave 26.3 g (81%) of cyclopentylmethyl chloroformate. Bp17-20 82°-84° C., nD21 1.4541. Analysis for C7H11ClO2. Found (calculated): Cl 21.37 (21.80). IR (neat) cm-1 : 1790 (CO).

후처리

  1. temperaturecooled to -5° to +5° C
  2. additionAfter the addition the reaction mixture
  3. customto attain room temperature
  4. filtrationThe precipitate was filtered off
  5. customthe solvent was evaporated
  6. distillationDistillation in vacuo

출처 및 근거

ORD 기록
ord-78f41280963744eb9868be20498626a4
출처 데이터셋
uspto-grants-1983_05
특허 번호
US04386081

반응 노트

불러오는 중…