Lawesson's reagent → 4,4,4-Trifluorobutanethioamide

HRID 570742ノート

反応式

HRID 570742 の反応式
[F:1][C:2]([F:9])([F:8])[CH2:3][CH2:4][C:5]([NH2:7])=O.COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:19]2)=CC=1>C1(C)C=CC=CC=1>[F:1][C:2]([F:9])([F:8])[CH2:3][CH2:4][C:5](=[S:19])[NH2:7]

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 12725184,4,4-Trifluorobutanamide

生成物 1

HCID 537527964,4,4-Trifluorobutanethioamide収率 73.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
80 °C

実験手順

A mixture of 4,4,4-trifluorobutanamide (17.9 g), 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide (51.3 g) and toluene (400 mL) was stirred at 80° C. for 3 hr. The reaction mixture was purified by aminopropylsilane-bonded silica gel column chromatography (ethyl acetate), and again purified by aminopropylsilane-bonded silica gel column chromatography (ethyl acetate/hexane) to give the title compound (14.6 g) as a solid.

後処理

  1. customThe reaction mixture was purified by aminopropylsilane-
  2. customagain purified by aminopropylsilane-

出典と根拠

ORDレコード
ord-817a1fb486f046d49147f73a70abb3d0
出典データセット
uspto-grants-2015_05
特許番号
US09023858B2

反応ノート

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