Hydrochloric Acid → HCID 67970562, 화합물

HRID 889535노트

반응식

HRID 889535 반응식
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([CH:13]([F:15])[F:14])=[C:7]([CH:12]=1)[C:8]([O:10][CH3:11])=[O:9])#[N:2].[ClH:16].[H][H]>[Pd].CO>[ClH:16].[NH2:2][CH2:1][C:3]1[CH:4]=[CH:5][C:6]([CH:13]([F:14])[F:15])=[C:7]([CH:12]=1)[C:8]([O:10][CH3:11])=[O:9]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 67970696HCID 67970696, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 67970562HCID 67970562, 화합물수율 83%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

Purge a mixture of methyl 5-cyano-2-(difluoromethyl)benzoate (9.37 g, 44.4 mmol, 1.0 equiv), palladium (10% on carbon, 3.00 g, 2.82 mmol, 0.064 equiv), and methanol (50 mL) with nitrogen, then add hydrochloric acid (37 wt % aqueous, 8.0 mL, 105.6 mmol, 2.38 equiv), and stir the resulting suspension under 275 kPaG of hydrogen at room temperature overnight. Remove the solids by filtration, concentrate the filtrate under reduced pressure, and dry the resulting material in a 40° C. vacuum oven overnight to give the title compound as a light brown solid (7.01 g, 83%). MS (m/z) 216 (M+1).

후처리

  1. customPurge
  2. customRemove the solids
  3. filtrationby filtration
  4. concentrationconcentrate the filtrate under reduced pressure
  5. customdry the resulting material in a 40° C. vacuum oven overnight

출처 및 근거

ORD 기록
ord-d81194d3ad3445abae548a18128aa598
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08252831B2

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