Lawesson's reagent → 2,3-Difluoro-4-(trifluoromethyl)benzene-1-carbothioamide

HRID 1767969ノート

反応式

HRID 1767969 の反応式
[F:1][C:2]1[C:10]([F:11])=[C:9]([C:12]([F:15])([F:14])[F:13])[CH:8]=[CH:7][C:3]=1[C:4]([NH2:6])=O.COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:25]2)=CC=1>O1CCCC1>[F:1][C:2]1[C:10]([F:11])=[C:9]([C:12]([F:15])([F:14])[F:13])[CH:8]=[CH:7][C:3]=1[C:4]([NH2:6])=[S:25]

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 27742332,3-Difluoro-4-(trifluoromethyl)benzamide

生成物 1

HCID 236144852,3-Difluoro-4-(trifluoromethyl)benzene-1-carbothioamide収率 186.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
130 °C

実験手順

A suspension of 2,3-difluoro-4-trifluoromethyl-benzamide (1 g, 4.4 mmol) and 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (Lawesson's reagent; 900 mg, 2.2 mmol) in tetrahydrofuran (2 ml) was stirred under microwave irradiation at 130° C. for 15 min. The solvent was removed under reduced pressure to give an orange oil which was purified by column chromatography (silica gel, heptane/AcOEt) to yield 1.0 g (4.1 mmol, 93%) of the title compound as yellow crystals.

後処理

  1. customThe solvent was removed under reduced pressure
  2. customto give an orange oil which
  3. customwas purified by column chromatography (silica gel, heptane/AcOEt)

出典と根拠

ORDレコード
ord-dca064b78e2446449994d664c1116ba0
出典データセット
uspto-grants-2007_06
特許番号
US07235572B2

反応ノート

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