Phosphorus sulfide (P2S5) → 3,4-Difluorobenzene-1-carbothioamide

HRID 554857노트

반응식

HRID 554857 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[F:11])[C:5]([NH2:7])=O.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:13]>C(OCC)C>[F:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[F:11])[C:5]([NH2:7])=[S:13]

참가 물질

4

반응물 2

HCID 14817Phosphorus sulfide (P2S5)HCID 5228323,4-Difluorobenzamide

생성물 1

HCID 167714643,4-Difluorobenzene-1-carbothioamide수율 100.8%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

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온도
0 °C

실험 절차

Dissolve 3,4-difluorobenzamide (4.95 g, 31.5 mmol) in diethyl ether (70 mL) and cool the mixture to 0° C. Add phosphorus pentasulfide (7.0 g, 31.5 mmol) and warm the mixture to room temperature overnight. Filter the mixture and concentrate the filtrate to obtain 5.5 g (100%) of a yellow solid. 1H NMR (300 MHz, DMSO-d6) δ: 9.99 (bs, 1H), 9.54 (bs, 1H), 7.89 (m, 1H), 7.75 (m, 1H), 7.46 (m, 1H).

후처리

  1. filtrationFilter the mixture
  2. concentrationconcentrate the filtrate

출처 및 근거

ORD 기록
ord-45e24c302a8c4f20bdbfa485e1bbf047
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08049013B2

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