Hydrochloric Acid → 4-Methylthiobenzyl alcohol methanesulfonate

HRID 850250노트

반응식

HRID 850250 반응식
[CH3:1][S:2][C:3]1[CH:10]=[CH:9][C:6]([CH2:7][OH:8])=[CH:5][CH:4]=1.[CH3:11][S:12](Cl)(=[O:14])=[O:13].C(N(CC)CC)C.Cl>C1(C)C=CC=CC=1>[CH3:11][S:12]([O:8][CH2:7][C:6]1[CH:9]=[CH:10][C:3]([S:2][CH3:1])=[CH:4][CH:5]=1)(=[O:14])=[O:13]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 592968[4-(Methylsulfanyl)phenyl]methanol

생성물 1

HCID 543237644-Methylthiobenzyl alcohol methanesulfonate수율 80.7%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
10 °C

실험 절차

In a sulfonating flask, 50 g (0.32 mol) of 4-methylthiobenzyl alcohol and 46.3 g (0.32 mol) of methylsulfonyl chloride are dissolved in 250 ml of toluene and, with cooling at 10° C., 32.5 g (0.32 mol) of triethylamine are added dropwise. The reaction mixture is then heated to room temperature and stirred overnight. 400 ml of 2N hydrochloric acid are then added to the reaction solution slowly and with cooling. The phases are separated and the organic phase is washed with water, dried over MgSO4 and concentrated in a rotary evaporator. 60 g (80%) of 4-methylthiobenzyl alcohol methanesulfonate are obtained in the form of a yellow oil.

후처리

  1. temperatureThe reaction mixture is then heated to room temperature
  2. temperaturewith cooling
  3. customThe phases are separated
  4. washthe organic phase is washed with water
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in a rotary evaporator

출처 및 근거

ORD 기록
ord-ea819aaf204143cc9fc2fdc2d2f8d40d
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06017675

반응 노트

불러오는 중…