Hydrochloric Acid → HCID 67970562、化合物

HRID 241439ノート

反応式

HRID 241439 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 MeOH (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% yield). ES/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. customand dry the resulting material in a 40° C. vacuum oven overnight

出典と根拠

ORDレコード
ord-072d06f217394903b25797486c687845
出典データセット
uspto-grants-2014_02
特許番号
US08648200B2

反応ノート

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