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Naphthalene → HCID 18001048, 화합물

HRID 441233
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HRID 441233 반응식
C1C2C(=CC=CC=2)C=CC=1.[Na].[Cl:12][C:13]1[CH:14]=[CH:15][C:16]2[N:22](S(C3C=CC(C)=CC=3)(=O)=O)[CH2:21][CH2:20][CH2:19][CH:18]([CH2:33][C:34]([O:36][CH2:37][CH3:38])=[O:35])[C:17]=2[CH:39]=1>C(COC)OC>[Cl:12][C:13]1[CH:14]=[CH:15][C:16]2[NH:22][CH2:21][CH2:20][CH2:19][CH:18]([CH2:33][C:34]([O:36][CH2:37][CH3:38])=[O:35])[C:17]=2[CH:39]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 931NaphthaleneHCID 5360545SodiumHCID 22405061HCID 22405061, 화합물

생성물 1

HCID 18001048HCID 18001048, 화합물수율 36.8%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매2회

실험 절차

To a solution of naphthalene (15.5 g) in dimethoxyethane (100 ml) was added sodium metal (2.79 g) in portions at 0° C. and the solution was stirred at the same temperature for 1 hour. The naphthilide was added to a solution of 7-chloro -5-ethoxycarbonylmethyl-1-(p-toluenesulfonyl)-2,3,4,5-tetrahydro-1H-1-benzazepine (9.89 g) in dimethoxyethane (400 ml) at -60° C. and the solution was stirred at the same temperature for 30 minutes. The reaction mixture was quenched with water and the solution was extracted with chloroform. The extract was washed with brine and dried over magnesium sulfate. The solvent was evaporated in vacuo to give an oil and the crude oil was purified by silica gel column to give 7-chloro-5-ethoxycarbonylmethyl -2,3,4,5-tetrahydro-1H-1-benzazepine (2.31 g).

후처리

  1. stirringthe solution was stirred at the same temperature for 30 minutes
  2. customThe reaction mixture was quenched with water
  3. extractionthe solution was extracted with chloroform
  4. washThe extract was washed with brine
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was evaporated in vacuo
  7. customto give an oil
  8. customthe crude oil was purified by silica gel column

출처 및 근거

ORD 기록
ord-97057135d9fd449496cc24f86fdf4047
출처 데이터셋
uspto-grants-1996_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05521170

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