Triethylamine → 2-(2-Chlorophenyl)ethyl methanesulfonate

HRID 440934

반응식

HRID 440934 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][CH2:9][OH:10].C(N(CC)CC)C.[CH3:18][S:19](Cl)(=[O:21])=[O:20]>O1CCCC1>[CH3:18][S:19]([O:10][CH2:9][CH2:8][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[Cl:1])(=[O:21])=[O:20]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 88266o-Chlorophenethylic alcohol

생성물 1

HCID 218880872-(2-Chlorophenyl)ethyl methanesulfonate수율 98.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 5.26 mL (40 mMol) 2-(2-chlorophenyl)ethanol and 8.36 mL (60 mMol) triethylamine in 100 mL tetrahydrofuran were added dropwise 3.25 mL (42 mMol) methanesulfonyl chloride with cooling. The reaction mixture was stirred 4 hours at ambient and was then concentrated under reduced pressure. The residue was partitioned between dichloromethane and water. The organic phase was separated and washed sequentially with water and saturated aqueous sodium chloride. The remaining organics were dried over sodium sulfate and concentrated under reduced pressure to give 9.22 gm (98.3%) of the title compound as a yellow oil. The product was used without further purification.

후처리

  1. temperaturewith cooling
  2. concentrationwas then concentrated under reduced pressure
  3. customThe residue was partitioned between dichloromethane and water
  4. customThe organic phase was separated
  5. washwashed sequentially with water and saturated aqueous sodium chloride
  6. dry with materialThe remaining organics were dried over sodium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-71731d44936e4ba7b5b4d009fd53129c
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05521197

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