Benzyl[3-(aminocarbonyl)-5-(2,4-difluorophenyl)-2-thienyl]carbamate → 2-Amino-5-(2,4-difluorophenyl)thiophene-3-carboxamide

HRID 385696ノート

反応式

HRID 385696 の反応式
C(OC(=O)[NH:10][C:11]1[S:12][C:13]([C:19]2[CH:24]=[CH:23][C:22]([F:25])=[CH:21][C:20]=2[F:26])=[CH:14][C:15]=1[C:16]([NH2:18])=[O:17])C1C=CC=CC=1.[H][H]>[Pd].C(O)C>[NH2:10][C:11]1[S:12][C:13]([C:19]2[CH:24]=[CH:23][C:22]([F:25])=[CH:21][C:20]=2[F:26])=[CH:14][C:15]=1[C:16]([NH2:18])=[O:17]

参加物

5

反応物 2

HCID 59526381Benzyl[3-(aminocarbonyl)-5-(2,4-difluorophenyl)-2-thienyl]carbamateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 595262952-Amino-5-(2,4-difluorophenyl)thiophene-3-carboxamide

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A suspension of benzyl[3-(aminocarbonyl)-5-(2,4-difluorophenyl)-2-thienyl]carbamate (240 mg, 0.618 mmol) and 10% palladium on carbon (326 mg, 0.306 mmol) in ethanol (130 mL) was placed under a hydrogen atmosphere by performing 5×15 second vacuum/hydrogen purge (supplied by balloon) fill cycles while vigorously stirring the mixture. The reaction was heated to reflux for 18 hours and then allowed to cool to ambient temperature. The suspension was filtered; the filtrate was collected and concentrated to yield the title compound as a light yellow solid.

後処理

  1. custompurge (supplied by balloon) fill cycles
  2. temperatureThe reaction was heated
  3. temperatureto reflux for 18 hours
  4. filtrationThe suspension was filtered
  5. customthe filtrate was collected
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-95a6580003ba427292fd01887558f7da
出典データセット
uspto-grants-2013_02
特許番号
US08367706B2

反応ノート

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