Phenyltrimethylammonium bromide dibromide → HCID 58495428, 화합물

HRID 516259노트

반응식

HRID 516259 반응식
[OH:1][C:2]1[CH:17]=[CH:16][C:5]2[CH2:6][CH2:7][N:8]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH2:9][CH2:10][C:4]=2[CH:3]=1.[Br-:18].[Br-].[Br-].C[N+](C)(C)C1C=CC=CC=1.C[N+](C)(C)C1C=CC=CC=1.C[N+](C)(C)C1C=CC=CC=1>ClCCl.CO>[Br:18][C:17]1[C:2]([OH:1])=[CH:3][C:4]2[CH2:10][CH2:9][N:8]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH2:7][CH2:6][C:5]=2[CH:16]=1

참가 물질

5

반응물 2

HCID 17977687Phenyltrimethylammonium bromide dibromideHCID 584953637-Hydroxy-1,2,4,5-tetrahydro-benzo[d]azepine-3-carboxylic acid ethyl ester

생성물 1

HCID 58495428HCID 58495428, 화합물수율 171%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

Under an argon atmosphere, to a mixed solution of 5.0 g of ethyl 7-hydroxy-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate in 100 ml of dichloromethane and 20 ml of methanol was added portionwise 8.05 g of N,N,N-trimethylanilinium tribromide under ice-cooling, followed by stirring at the same temperature for 1 hour. The reaction mixture was concentrated under reduced pressure, the residue was extracted by the addition of ethyl acetate and water, and the organic layer was washed with 1 M aqueous hydrochloric acid and saturated brine, dried over anhydrous magnesium sulfate, and then filtered, and the filtrate was concentrated under reduced pressure to obtain 6.67 g of ethyl 7-bromo-8-hydroxy-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate as a beige solid.

후처리

  1. temperaturecooling
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. extractionthe residue was extracted by the addition of ethyl acetate and water
  4. washthe organic layer was washed with 1 M aqueous hydrochloric acid and saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-f24c1da8e61b4a078f432902741e612c
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09108977B2

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