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Dichloromethane → HCID 19026199, 화합물

HRID 1033514
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HRID 1033514 반응식
[C:1](OC(=O)C)(=[O:3])[CH3:2].[C:8]1([CH2:14][O:15][NH:16][CH:17]2[CH2:26][CH2:25][CH2:24][C:23]3[N:22]=[C:21]([O:27][CH2:28][C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)[CH:20]=[CH:19][C:18]2=3)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[Cl:35]CCl>>[ClH:35].[C:8]1([CH2:14][O:15][N:16]([CH:17]2[CH2:26][CH2:25][CH2:24][C:23]3[N:22]=[C:21]([O:27][CH2:28][C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)[CH:20]=[CH:19][C:18]2=3)[C:1](=[O:3])[CH3:2])[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6344Dichloromethane2회HCID 7918Acetic AnhydrideHCID 19026180HCID 19026180, 화합물

생성물 1

HCID 19026199HCID 19026199, 화합물수율 52%

실험 절차

Acetic anhydride (3.77 g) was added to a solution of N,N-dimethylaminopyridine (0.2 g), N,2-bis(phenylmethoxy)-5,6,7,8-tetrahydro-5-quinolinamine (12.1 g) and dichloromethane (170 ml) at room temperature. The mixture was stirred at room temperature for 48 hrs, diluted with dichloromethane, and extracted with saturated sodium bicarbonate solution. The combined extracts were washed with water, brine, dried over anhydrous magnesium sulfate, filtered, and the filtrate was concentrated. The residue was dissolved in methanol and acidified with 2-propanol/hydrochloric acid solution. The mixture was evaporated and the residue was recrystallized from ethanol/ethyl acetate to give 7.64 g (52%) of product, mp 125°-126° C.

후처리

  1. extractionextracted with saturated sodium bicarbonate solution
  2. washThe combined extracts were washed with water, brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated
  6. dissolutionThe residue was dissolved in methanol
  7. customThe mixture was evaporated
  8. customthe residue was recrystallized from ethanol/ethyl acetate

출처 및 근거

ORD 기록
ord-a98cee29685e4b1bbd77c0da95a34a85
출처 데이터셋
uspto-grants-1994_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05310914

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