Water → 4-[(2-Chloro-6,11-dihydro-5H-dibenz[b,e]azepin-5-yl) carbonyl]phenyl-2-methylbenzamide

HRID 1456251ノート

反応式

HRID 1456251 の反応式
[Cl:1][C:2]1[CH:25]=[CH:24][C:5]2[N:6]([C:15](=[O:23])[C:16]3[CH:21]=[CH:20][C:19](N)=[CH:18][CH:17]=3)[CH2:7][C:8]3[CH:14]=[CH:13][CH:12]=[CH:11][C:9]=3[CH2:10][C:4]=2[CH:3]=1.C([N:28](CC)CC)C.[CH3:33][C:34]1[CH:42]=[CH:41][CH:40]=[CH:39][C:35]=1[C:36](Cl)=[O:37].O>ClCCl>[Cl:1][C:2]1[CH:25]=[CH:24][C:5]2[N:6]([C:15]([C:16]3[CH:21]=[CH:20][C:19]([C:42]4[C:34]([CH3:33])=[C:35]([CH:39]=[CH:40][CH:41]=4)[C:36]([NH2:28])=[O:37])=[CH:18][CH:17]=3)=[O:23])[CH2:7][C:8]3[CH:14]=[CH:13][CH:12]=[CH:11][C:9]=3[CH2:10][C:4]=2[CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 702762-Methylbenzoyl chlorideHCID 544045372-Chloro-5-(4-aminobenzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine

生成物 1

HCID 867515734-[(2-Chloro-6,11-dihydro-5H-dibenz[b,e]azepin-5-yl) carbonyl]phenyl-2-methylbenzamide収率 68.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 0.349 g of 2-chloro-5-(4-aminobenzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine, 0.131 g of triethylamine and 0.201 g of 2-methylbenzoyl chloride in 13 ml of dichloromethane is stirred at room temperature for 3 hours. The mixture is poured into water and the organic layer separated. The organic layer is washed with 1N HCl, H2O, 1N NaHCO3, brine and dried (Na2 SO4). The solution is filtered through a thin pad of hydrous magnesium silicate and the pad washed with dichloromethane. The filtrate is concentrated and the solid crystallized from dichloromethane-hexane to give 0.32 g of crystals, m.p. 187°-189° C.

後処理

  1. customthe organic layer separated
  2. washThe organic layer is washed with 1N HCl, H2O, 1N NaHCO3, brine
  3. customdried (Na2 SO4)
  4. filtrationThe solution is filtered through a thin pad of hydrous magnesium silicate
  5. washthe pad washed with dichloromethane
  6. concentrationThe filtrate is concentrated
  7. customthe solid crystallized from dichloromethane-hexane

出典と根拠

ORDレコード
ord-8a5da8bc73fe4b0f81f0aab358ac8304
出典データセット
uspto-grants-1998_12
特許番号
US05843952

反応ノート

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