Methanesulfonyl chloride → (2'-Chloro-3-methylbiphenyl-4-yl)methyl methanesulfonate

HRID 2194881노트

반응식

HRID 2194881 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][C:11]([CH2:14][OH:15])=[C:10]([CH3:16])[CH:9]=1.C(N(C(C)C)CC)(C)C.[CH3:26][S:27](Cl)(=[O:29])=[O:28]>C(Cl)Cl.O>[CH3:26][S:27]([O:15][CH2:14][C:11]1[CH:12]=[CH:13][C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[Cl:1])=[CH:9][C:10]=1[CH3:16])(=[O:29])=[O:28]

참가 물질

6

반응물 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 67448566(2'-Chloro-3-methylbiphenyl-4-yl)methanol

생성물 1

HCID 86658848(2'-Chloro-3-methylbiphenyl-4-yl)methyl methanesulfonate

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

To a solution of (2′-chloro-3-methylbiphenyl-4-yl)methanol from step 1 in CH2Cl2 (0.13M) at 0° C. was added diisopropyl ethylamine (1.5 eq.) then methanesulfonyl chloride (1.1 eq.). The reaction mixture was stirred at room temperature for 2 h, poured in water and extracted with EtOAc. The organic extract was washed with water, brine, dried over MgSO4 filtered and concentrated to afford the title compound which was used as such in the next step.

후처리

  1. extractionextracted with EtOAc
  2. extractionThe organic extract
  3. washwas washed with water, brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-4e3be230bca0449c922820128be7d0df
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08334308B2

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