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

HRID 2194881ノート

反応式

HRID 2194881 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-4e3be230bca0449c922820128be7d0df
出典データセット
uspto-grants-2012_12
特許番号
US08334308B2

反応ノート

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