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

HRID 1767969노트

반응식

HRID 1767969 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
130 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-dca064b78e2446449994d664c1116ba0
출처 데이터셋
uspto-grants-2007_06
특허 번호
US07235572B2

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