Methyl triflate → Methyl-tetrahydrothiopyran-4-one triflate

HRID 43295

反応式

HRID 43295 の反応式
[S:1]1[CH2:6][CH2:5][C:4](=[O:7])[CH2:3][CH2:2]1.[CH3:8][O:9][S:10]([C:13]([F:16])([F:15])[F:14])(=[O:12])=[O:11]>ClCCl>[OH:12][S:10]([C:13]([F:16])([F:15])[F:14])(=[O:11])=[O:9].[CH3:8][CH:2]1[CH2:3][C:4](=[O:7])[CH2:5][CH2:6][S:1]1

参加物

4

反応物 2

HCID 9526Methyl triflateHCID 66173Tetrahydrothiopyran-4-one

生成物 1

HCID 87658744Methyl-tetrahydrothiopyran-4-one triflate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2 mmol of tetrahydrothiopyran-4-one was dissolved in 5 ml of dichloromethane at 0° C., and about 2 mmol of methyltrifluoromethane sulfonate was slowly dripped to the mixture. The solvent was removed after about 30 minutes, and was then recrystallized with a mixture of ethyl acetate and hexane (1:2 by weight) to obtain a white solid product. The solid product was filtered and dried for 1 hour in an oven at 50° C. to obtain the following product:

後処理

  1. customThe solvent was removed after about 30 minutes
  2. customwas then recrystallized with a mixture of ethyl acetate and hexane (1:2 by weight)
  3. customto obtain a white solid product
  4. filtrationThe solid product was filtered
  5. customdried for 1 hour in an oven at 50° C.
  6. customto obtain the following product

出典と根拠

ORDレコード
ord-e251509fdc3047e78ec0d2f448c09308
出典データセット
uspto-grants-2013_09
特許番号
US08536347B2

関連ノート

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