Sodium Hydroxide → HCID 22990165、化合物

HRID 1169425ノート

反応式

HRID 1169425 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]=[CH:10][C:11]3[O:17][CH2:16][CH2:15][C:14]([C:18]([N:20]4[CH2:25][CH2:24][CH:23]([NH:26]C(=O)C(F)(F)F)[CH2:22][CH2:21]4)=[O:19])=[CH:13][C:12]=3[CH:33]=2)=[CH:4][CH:3]=1.[OH-].[Na+]>CO>[NH2:26][CH:23]1[CH2:24][CH2:25][N:20]([C:18]([C:14]2[CH2:15][CH2:16][O:17][C:11]3[CH:10]=[CH:9][C:8]([C:5]4[CH:6]=[CH:7][C:2]([CH3:1])=[CH:3][CH:4]=4)=[CH:33][C:12]=3[CH:13]=2)=[O:19])[CH2:21][CH2:22]1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 229900891-(7-(4-Methylphenyl)-2,3-dihydro-1-benzooxepine-4-carbonyl)-4-trifluoroacetamidopiperidine

生成物 1

HCID 22990165HCID 22990165、化合物収率 87%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To 1-(7-(4-methylphenyl)-2,3-dihydro-1-benzooxepine-4-carbonyl)-4-trifluoroacetamidopiperidine (1.6 g) dissolved in methanol (100 ml) was added a 1 N aqueous solution of sodium hydroxide (7 ml), and the resulting mixture was stirred at room temperature overnight. The reaction mixture was concentrated and was then extracted with ethyl acetate. The organic layer was washed with water and an aqueous saturated solution of sodium chloride, and was then dried with anhydrous magnesium sulfate. The resulting organic layer was evaporated under reduced pressure to remove the solvent to obtain crude crystals. The crude crystals were recrystallized from ethyl acetate/hexane to obtain 4-amino-1-(7-(4-methylphenyl)-2,3-dihydro-1-benzooxepine-4-carbonyl)piperidine (compound 76) (1.1 g) as colorless prisms.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. extractionwas then extracted with ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materialan aqueous saturated solution of sodium chloride, and was then dried with anhydrous magnesium sulfate
  5. customThe resulting organic layer was evaporated under reduced pressure
  6. customto remove the solvent
  7. customto obtain crude crystals
  8. customThe crude crystals were recrystallized from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-6e7641c33df34888844a5af7c2b9c833
出典データセット
uspto-grants-2003_09
特許番号
US06627651B1

反応ノート

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