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4-Toluenesulfonyl chloride → 1-Benzyl-8-methoxy-4,5-dihydro-1H-benzo[C]azepin-3(2H)-one

HRID 625926
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HRID 625926 반응식
C1(C)C=CC(S(Cl)(=O)=[O:8])=CC=1.C(N(CC)CC)C.CN(C1C=CC=CN=1)C.[CH2:28]([CH:35]1[C:44]2[C:39](=[CH:40][CH:41]=[C:42]([O:45][CH3:46])[CH:43]=2)[CH2:38][CH2:37][C:36]1=[N:47]O)[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1>ClCCl>[CH2:28]([CH:35]1[C:44]2[CH:43]=[C:42]([O:45][CH3:46])[CH:41]=[CH:40][C:39]=2[CH2:38][CH2:37][C:36](=[O:8])[NH:47]1)[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.[CH2:28]([CH:35]1[C:44]2[CH:43]=[C:42]([O:45][CH3:46])[CH:41]=[CH:40][C:39]=2[CH2:38][CH2:37][NH:47][C:36]1=[O:8])[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 218852-DimethylaminopyridineHCID 86674675HCID 86674675, 화합물

생성물 2

HCID 709822691-Benzyl-8-methoxy-4,5-dihydro-1H-benzo[C]azepin-3(2H)-one수율 67%HCID 710870541-benzyl-8-methoxy-4,5-dihydro-1H-benzo[d]azepin-2(3H)-one
수율 26%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

To a solution of 8.46 mmol of p-toluenesulfonylchloride, 8.4 mmol triethylamine and 0.16 mmol of dimethylaminopyridine in 5 ml of dichloromethane was added a solution of 945 mg of 1-benzyl-7-methoxy-3,4-dihydronaphthalen-2(1H)-one oxime in 5 ml dichloromethane. The solution was stirred at room temperature over night. The mixture was diluted with dichloromethane and washed with water and saturated NaHCO3 solution. The combined organic layers were dried over MgSO4 and filtered. Evaporation of the solvent gave 1.9 g of crude material that was purified by flash chromatography to yield 637 mg of the desired isomer 1-benzyl-8-methoxy-4,5-dihydro-1H-benzo[c]azepin-3(2H)-one (67%) and 248 mg of its regioisomer 1-benzyl-8-methoxy-4,5-dihydro-1H-benzo[d]azepin-2(3H)-one (26%).

후처리

  1. washwashed with water and saturated NaHCO3 solution
  2. dry with materialThe combined organic layers were dried over MgSO4
  3. filtrationfiltered
  4. customEvaporation of the solvent
  5. customgave 1.9 g of crude material that
  6. customwas purified by flash chromatography

출처 및 근거

ORD 기록
ord-7112cf6e84e1409f9abc57fda04ff649
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09309200B2

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