N,N-二甲基甲酰胺 → 137976-09-1

HRID 1340

反应方程式

HRID 1340 反应方程式
[N+:1]([C:4]1[CH:23]=[CH:22][C:7]([C:8]([N:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[C:14](=[O:21])[CH2:13][CH2:12][CH2:11]2)=[O:9])=[CH:6][CH:5]=1)([O-])=O.CN(C)C=O>[Ni].CO>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]([C:8]([N:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[C:14](=[O:21])[CH2:13][CH2:12][CH2:11]2)=[O:9])=[CH:22][CH:23]=1

参与物

5

反应物 2

HCID 6228N,N-二甲基甲酰胺HCID 107337295H-1-Benzazepin-5-one, 1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-

产物 1

HCID 10707874137976-09-1

试剂、催化剂与溶剂 2

HCID 935Nickel催化剂HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂

实验过程

A 19.2 g portion of 1-(4-nitrobenzoyl)-2,3,4,5-tetrahydro1H-1-benzazepin-5-one was dissolved in a mixed solvent consisting of 200 ml of dimethylformamide and 100 ml of methyl alcohol, and 3 ml of Raney nickel was added to the resulting solution to carry out hydrogenation at normal pressure. After completion of the hydrogen absorption, the reaction solution was filtered and concentrated. The thus obtained residue was dissolved in dichloromethane and then washed with a saturated sodium bicarbonate aqueous solution. The resulting dichloromethane layer was dried over anhydrous magnesium sulfate and then concentrated under a reduced pressure. The thus obtained residue was recrystallized from methyl alcohol to obtain 15.5 g of 1-(4-aminobenzoyl)-2,3,4,5-tetrahydro1H-1-benzazepin-5-one.

后处理

  1. additionwas added to the resulting solution
  2. customAfter completion of the hydrogen absorption
  3. filtrationthe reaction solution was filtered
  4. concentrationconcentrated
  5. dissolutionThe thus obtained residue was dissolved in dichloromethane
  6. washwashed with a saturated sodium bicarbonate aqueous solution
  7. dry with materialThe resulting dichloromethane layer was dried over anhydrous magnesium sulfate
  8. concentrationconcentrated under a reduced pressure
  9. customThe thus obtained residue was recrystallized from methyl alcohol

来源与证据

ORD记录
ord-ef4bb1c6c9b74f7baca312f5b2f73584
来源数据集
uspto-grants-1998_03
专利号
US05723606

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