Methanesulfonyl chloride → HCID 86610159、化合物

HRID 1363213ノート

反応式

HRID 1363213 の反応式
[C:1]1([C@H:7]2[CH2:12][C@@H:11]([OH:13])[CH2:10][CH2:9][O:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CCN(C(C)C)C(C)C.[CH3:23][S:24](Cl)(=[O:26])=[O:25]>C(Cl)Cl>[CH3:23][S:24]([O:13][C@H:11]1[CH2:10][CH2:9][O:8][C@@H:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH2:12]1)(=[O:26])=[O:25]

参加物

5

反応物 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 11423901cis-2-phenyltetrahydro-2H-pyran-4-ol

生成物 1

HCID 86610159HCID 86610159、化合物収率 62.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of cis-2-phenyltetrahydro-2H-pyran-4-ol (1 g) in DCM (20 mL) was cooled in an ice-salt water bath and treated with DIEA (2.2 g) and methanesulfonyl chloride (0.7 g) for 2 hours. The mixture was diluted with DCM (50 mL) and washed with water and brine. The organic layer was dried and concentrated. Preparative TLC provided 0.9 g of cis-2-phenyl-tetrahydro-2H-pyran-4-yl methanesulfonate.

後処理

  1. washwashed with water and brine
  2. customThe organic layer was dried
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-8d10b390854d49fe90b5c7f587dbb0c7
出典データセット
uspto-grants-2011_02
特許番号
US07884109B2

反応ノート

読み込み中…