Hydrochloric Acid → HCID 67970562、化合物

HRID 889535ノート

反応式

HRID 889535 の反応式
[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]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 67970696HCID 67970696、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 67970562HCID 67970562、化合物収率 83%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d81194d3ad3445abae548a18128aa598
出典データセット
uspto-grants-2012_08
特許番号
US08252831B2

反応ノート

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