Ethyl bromoacetate → HCID 53861417, 화합물

HRID 1683763노트

반응식

HRID 1683763 반응식
[H-].[K+].[Cl:3][C:4]1[C:9]2[CH2:10][CH2:11][N:12]([CH3:15])[CH2:13][CH2:14][C:8]=2[C:7]([OH:16])=[CH:6][CH:5]=1.Br[CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20]>CN(C)C=O>[Cl:3][C:4]1[C:9]2[CH2:10][CH2:11][N:12]([CH3:15])[CH2:13][CH2:14][C:8]=2[C:7]([O:16][CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])=[CH:6][CH:5]=1

참가 물질

5

반응물 3

HCID 7748Ethyl bromoacetateHCID 82127Potassium hydrideHCID 133383339-Chloro-3-methyl-2,3,4,5-tetrahydro-1H-3-benzazepin-6-ol

생성물 1

HCID 53861417HCID 53861417, 화합물수율 76%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A 35% dispersion of potassium hydride in mineral oil (2.6 g, 23 mmol) in dimethylformamide (40 ml) was stirred and treated with 9-chloro-2,3,4,5-tetrahydro-3-methyl-1H-3-benzazepin-6-ol (4.0 g, 19 mmol), stirred for 20 minutes, treated with ethyl bromoacetate (3.8 g, 23 mmol) and stirred for 72 hours. The mixture was concentrated, partitioned between water and methylene chloride and the organic phase was washed, dried with magnesium sulfate and concentrated. The residue was chromatographed on silica gel eluted with methanol-methylene chloride (8:92) to give 4.3 g of ethyl [(9-chloro-2,3,4,5-tetrahydro-3-methyl-1H-3-benzazepin-6-yl)oxy]acetate.

후처리

  1. stirringstirred for 72 hours
  2. concentrationThe mixture was concentrated
  3. custompartitioned between water and methylene chloride
  4. washthe organic phase was washed
  5. dry with materialdried with magnesium sulfate
  6. concentrationconcentrated
  7. customThe residue was chromatographed on silica gel
  8. washeluted with methanol-methylene chloride (8:92)

출처 및 근거

ORD 기록
ord-8c6351e952dd4a23978145d5122f121a
출처 데이터셋
uspto-grants-1997_06
특허 번호
US05639748

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