Triethylamine → HCID 88117526, 화합물

HRID 1169427노트

반응식

HRID 1169427 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]([CH:18]=O)=[CH:13][C:12]=3[CH:20]=2)=[CH:4][CH:3]=1.[F:21][C:22]([F:33])([F:32])[C:23]([NH:25][CH:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1)=[O:24].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(N(CC)CC)C>ClCCCl>[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]([CH2:18][N:29]4[CH2:30][CH2:31][CH:26]([NH:25][C:23](=[O:24])[C:22]([F:21])([F:32])[F:33])[CH2:27][CH2:28]4)=[CH:13][C:12]=3[CH:20]=2)=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 5049666Sodium triacetoxyborohydride2회HCID 107742532,2,2-trifluoro-N-(piperidin-4-yl)acetamideHCID 229901807-(4-Methylphenyl)-2,3-dihydro-1-benzooxepine-4-carbaldehyde

생성물 1

HCID 88117526HCID 88117526, 화합물

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

To 7-(4-methylphenyl)-2,3-dihydro-1-benzooxepine-4-carbaldehyde (2.0 g) and 4-trifluoroacetamidopiperidine (1.56 g) dissolved in 1,2-dichloroethane (50 ml) was added under ice cooling sodium triacetoxyborohydride (1.8 g), and the resulting mixture was stirred at room temperature overnight under a nitrogen atmosphere. Thereto were added triethylamine (1.1 ml) and sodium triacetoxyborohydride (0.8 g), and the resulting mixture was stirred at room temperature overnight under a nitrogen atmosphere. The reaction mixture was evaporated to remove the solvent, was neutralized with a 1 N aqueous solution of sodium hydrogen carbonate and was extracted with ethyl acetate. The organic layer was washed with water and an aqueous saturated solution of sodium chloride, and then was dried with anhydrous magnesium sulfate. The resulting organic layer was evaporated under reduced pressure to remove the solvent to obtain crude crystals (3.0 g). A portion of the crystals was recrystallized from ethyl acetate/hexane to obtain 1-(7-(4-methylphenyl)-2,3-dihydro-1-benzooxepin-4-ylmethy)-4-trifluoroacetamidopiperidine as light yellow crystals.

후처리

  1. additionwas added under ice
  2. stirringthe resulting mixture was stirred at room temperature overnight under a nitrogen atmosphere
  3. customThe reaction mixture was evaporated
  4. customto remove the solvent
  5. extractionwas extracted with ethyl acetate
  6. washThe organic layer was washed with water
  7. dry with materialan aqueous saturated solution of sodium chloride, and then was dried with anhydrous magnesium sulfate
  8. customThe resulting organic layer was evaporated under reduced pressure
  9. customto remove the solvent
  10. customto obtain crude crystals (3.0 g)
  11. customA portion of the crystals was recrystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-b5956ba290ea41259dbbbe97e3a8840f
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06627651B1

반응 노트

불러오는 중…