Urea → 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboxamide

HRID 35175

反応式

HRID 35175 の反応式
[CH:1]1[C:11]2[C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[CH2:8][NH:7][CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[NH2:16][C:17](N)=[O:18]>>[CH:1]1[C:11]2[C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[CH2:8][N:7]([C:17]([NH2:16])=[O:18])[CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1

参加物

3

反応物 2

HCID 1176UreaHCID 811835H-Dibenz(c,e)azepine, 6,7-dihydro-

生成物 1

HCID 200417145,7-dihydro-6H-dibenz[c,e]azepine-6-carboxamide

反応条件

温度
120 °C

実験手順

A mixture of 1.95 g of 6,7-dihydro-5H-dibenz[c,e]azepine and 3 g of urea is stirred at 120° C. for 15 minutes and then poured onto ice/water. After extracting the resulting aqueous mixture with methylene chloride the combined extracts are washed with water, dried over anhydrous sodium sulphate and evaporated. The solid residue is recrystallized from n-hexane/ethyl acetate, and in this manner there is obtained pure 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboxamide, m.p. 212°-214° C.

後処理

  1. additionpoured onto ice/water
  2. extractionAfter extracting the resulting aqueous mixture with methylene chloride the combined extracts
  3. washare washed with water
  4. dry with materialdried over anhydrous sodium sulphate
  5. customevaporated
  6. customThe solid residue is recrystallized from n-hexane/ethyl acetate

出典と根拠

ORDレコード
ord-57670e097dfc4a52a1ddf6e89ecb4ec1
出典データセット
uspto-grants-1988_08
特許番号
US04766115

関連ノート

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