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

HRID 1762712

반응식

HRID 1762712 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-5c60ab0e427b4cac80bc56d6f877f654
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04833245

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