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

HRID 35175

반응식

HRID 35175 반응식
[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

참가 물질

3

반응물 2

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

생성물 1

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

반응 조건

온도
120 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-57670e097dfc4a52a1ddf6e89ecb4ec1
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766115

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