Methanesulfonyl chloride → HCID 57706174、化合物

HRID 1662489ノート

反応式

HRID 1662489 の反応式
[CH3:1][C:2]([Si:5]([CH3:30])([CH3:29])[O:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[CH:19]=[C:18]([O:20][CH3:21])[CH:17]=[CH:16][C:15]=2[F:22])=[C:10]([CH:23](O)[C:24]([CH3:27])([CH3:26])[CH3:25])[CH:9]=1)([CH3:4])[CH3:3].CS([Cl:35])(=O)=O>C(Cl)Cl.O>[Cl:35][CH:23]([C:10]1[CH:9]=[C:8]([CH2:7][O:6][Si:5]([C:2]([CH3:4])([CH3:3])[CH3:1])([CH3:30])[CH3:29])[CH:13]=[CH:12][C:11]=1[C:14]1[CH:19]=[C:18]([O:20][CH3:21])[CH:17]=[CH:16][C:15]=1[F:22])[C:24]([CH3:27])([CH3:26])[CH3:25]

参加物

5

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 57705499HCID 57705499、化合物

生成物 1

HCID 57706174HCID 57706174、化合物収率 43.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of 69.16A (0.200 g, 0.46 mmol) in DCM (5.00 mL) at 0° C. was added TEA (0.077 mL, 0.55 mmol), followed by methanesulfonyl chloride (0.043 mL, 0.55 mmol). The reaction was then stirred for 22 hours, diluted with water, and extracted three times with EtOAc. After drying over anhydrous magnesium sulfate and filtering, the organic solvent was removed under reduced pressure and the product was purified on silica gel (0-10% EtOAc in hexanes) to yield 69.16B as a colorless oil (0.090 g, 43% yield) and a further product 69.16C as a clear oil (0.050 g, 21% yield).

後処理

  1. extractionextracted three times with EtOAc
  2. dry with materialAfter drying over anhydrous magnesium sulfate
  3. filtrationfiltering
  4. customthe organic solvent was removed under reduced pressure
  5. customthe product was purified on silica gel (0-10% EtOAc in hexanes)

出典と根拠

ORDレコード
ord-1098929f858f4111b528e192ac25845f
出典データセット
uspto-grants-2011_10
特許番号
US08030354B2

反応ノート

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