Triethylamine → HCID 13457150, 화합물

HRID 462423

반응식

HRID 462423 반응식
[C:1]([C:4]1[O:5][C:6]2[CH:12]=[CH:11][CH:10]=[CH:9][C:7]=2[CH:8]=1)(=[O:3])[CH3:2].BrBr.C(=O)(O)[O-].[Na+].[Cl:20][C:21]1[CH:26]=[C:25]([N:27]2[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]2)[CH:24]=[CH:23][C:22]=1[CH2:33][OH:34].C(N(CC)CC)C>CCOCC.CC(C)=O>[Cl:20][C:21]1[CH:26]=[C:25]([N:27]2[CH2:32][CH2:31][N:30]([CH2:2][C:1]([C:4]3[O:5][C:6]4[CH:12]=[CH:11][CH:10]=[CH:9][C:7]=4[CH:8]=3)=[O:3])[CH2:29][CH2:28]2)[CH:24]=[CH:23][C:22]=1[CH2:33][OH:34]

참가 물질

8

반응물 5

HCID 8471TriethylamineHCID 154352-AcetylbenzofuranHCID 24408BromineHCID 516892Sodium BicarbonateHCID 134571012-Chloro-4-(1-piperazinyl)benzenemethanol

생성물 1

HCID 13457150HCID 13457150, 화합물

시약·촉매·용매 2

HCID 180Acetone용매HCID 3283Diethyl Ether용매

실험 절차

A solution of 2-acetylbenzofuran (3.2 g. 0.02) in ether (50 ml) was treated with bromine (3.2 g., 0.02 mole) portionwise at room temperature. The mixture rapidly decolorized to a light yellow solution that was poured into cold aqueous sodium bicarbonate. The layers were separated and the aqueous layer was extracted with ether. The combined ether extracts were dried (K2CO3) and the ether was removed in vacuo, keeping the mixture cold. The gummy, off-white solid was dissolved in acetone (50 ml) and quickly added to a solution of 2-chloro-4-(1-piperazinyl)benzenemethanol (4.0 g, 0.0176 mole) and triethylamine (2.0 g, 0.902 mole) in acetone (200 ml). The mixture was stirred at room temperature for one hour, then cooled in an ice bath. The solid was collected, washed with ether, and air dried. Recrystallization from acetone-ethanol gave 3.7 g (55%), mp 169°-172°.

후처리

  1. customThe layers were separated
  2. extractionthe aqueous layer was extracted with ether
  3. dry with materialThe combined ether extracts were dried (K2CO3)
  4. customthe ether was removed in vacuo
  5. dissolutionThe gummy, off-white solid was dissolved in acetone (50 ml)
  6. temperaturecooled in an ice bath
  7. customThe solid was collected
  8. washwashed with ether, and air
  9. customdried
  10. customRecrystallization from acetone-ethanol
  11. customgave 3.7 g (55%), mp 169°-172°

출처 및 근거

ORD 기록
ord-4ad655b2ba1847409c22775831909eab
출처 데이터셋
uspto-grants-1985_05
특허 번호
US04515793

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