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

HRID 625926
ノート
印刷プレビュー

反応式

HRID 625926 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 218852-DimethylaminopyridineHCID 86674675HCID 86674675、化合物

生成物 2

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-7112cf6e84e1409f9abc57fda04ff649
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09309200B2

反応ノート

読み込み中…

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