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

HRID 1088379ノート

反応式

HRID 1088379 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b7fb063ae46e458998792f50178d65fa
出典データセット
uspto-grants-1990_10
特許番号
US04962115

反応ノート

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