Acetic Acid → HCID 22329115, 화합물

HRID 587091노트

반응식

HRID 587091 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][CH2:10][CH2:9][CH2:8][C:7](=[O:12])[C:6]=2[CH:13]=1.[CH:14](=O)[CH2:15][CH3:16].C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCCl.O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH2:14][CH2:15][CH3:16])[CH2:10][CH2:9][CH2:8][C:7](=[O:12])[C:6]=2[CH:13]=1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 527PropanalHCID 5049666Sodium triacetoxyborohydrideHCID 223291087-Bromo-1,2,3,4-tetrahydro-5H-1-benzazepin-5-one

생성물 1

HCID 22329115HCID 22329115, 화합물

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 962Water용매

실험 절차

To a solution of 7-bromo-2,3,4,5-tetrahydro-1H-1-benzazepine-5-one (5.0 g), propionaldehyde (15 ml) and acetic acid (4.7 ml) in 1,2-dichloroethane (250 ml) was added sodium triacetoxyborohydride (22.0 g) at room temperature, and the mixture was stirred for 6 hours. To the reaction system was added water, and the mixture was extracted with ethyl acetate. The organic layer was washed with an aqueous solution of sodium hydrogen carbonate and saturated brine, and dried with magnesium sulfate. After concentration under reduced pressure, the residue was separated and purified with column chromatography (ethyl acetate:hexane=1:4) to give 7-bromo-1-propyl-2,3,4,5-tetrahydro-1H-1-benzazepine-5-one (5.89 g) as yellow oil.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with an aqueous solution of sodium hydrogen carbonate and saturated brine
  3. dry with materialdried with magnesium sulfate
  4. concentrationAfter concentration under reduced pressure
  5. customthe residue was separated
  6. custompurified with column chromatography (ethyl acetate:hexane=1:4)

출처 및 근거

ORD 기록
ord-282eb1e0f185432a99174646bddc456b
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936602B1

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