Sodium Hydroxide → HCID 22990165, 화합물

HRID 1169425노트

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HRID 1169425 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 22990165HCID 22990165, 화합물수율 87%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6e7641c33df34888844a5af7c2b9c833
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06627651B1

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