Methanesulfonyl chloride → 2-(2,4-Dichlorophenoxy)-1-propanol methanesulfonate

HRID 1088379노트

반응식

HRID 1088379 반응식
[Cl:1][C:2]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:3]=1[O:4][CH:5]([CH3:8])[CH2:6][OH:7].[CH3:14][S:15](Cl)(=[O:17])=[O:16]>C(N(CC)CC)C>[CH3:14][S:15]([O:7][CH2:6][CH:5]([O:4][C:3]1[CH:9]=[CH:10][C:11]([Cl:13])=[CH:12][C:2]=1[Cl:1])[CH3:8])(=[O:17])=[O:16]

참가 물질

4

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 3509832-(2,4-Dichlorophenoxy)propan-1-ol

생성물 1

HCID 150969832-(2,4-Dichlorophenoxy)-1-propanol methanesulfonate

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

To a stirred mixture of 324 parts of 2-(2,4-dichloro-phenoxy)-1-propanol and 700 parts of N,N-diethylethanamine were added dropwise at room temperature 335 parts of methanesulfonyl chloride (exothermic reaction: the temperature roses to reflux temperature). While cooling in a water-bath, stirring was continued for 30 minutes at room temperature. The reaction mixture was poured onto water and the product was extracted with 2,2'-oxybispropane. The extract was dried, filtered and evaporated. The residue was distilled by vacuum distillation, yielding 300 parts of 2-(2,4-dichlorophenoxy)-1-propanol methanesulfonate (ester); bp. 130° C. at 2×10-4 mm. pressure (intermediate 101).

후처리

  1. customexothermic reaction
  2. temperaturethe temperature roses to reflux temperature)
  3. temperatureWhile cooling in a water-bath
  4. additionThe reaction mixture was poured onto water
  5. extractionthe product was extracted with 2,2'-oxybispropane
  6. customThe extract was dried
  7. filtrationfiltered
  8. customevaporated
  9. distillationThe residue was distilled by vacuum distillation

출처 및 근거

ORD 기록
ord-b7fb063ae46e458998792f50178d65fa
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04962115

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