Sodium Carbonate → ethyl 5,7-dihydro-6H-dibenz[c,e]azepine-6carboximidate

HRID 35171

반응식

HRID 35171 반응식
[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:16]([NH2:18])=[O:17])[CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.F[B-](F)(F)F.[CH2:24]([O+](CC)CC)[CH3:25].C(=O)([O-])[O-].[Na+].[Na+]>C(Cl)Cl>[CH:12]1[C:10]2[C:11]3[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=3[CH2:6][N:7]([C:16](=[NH:18])[O:17][CH2:24][CH3:25])[CH2:8][C:9]=2[CH:15]=[CH:14][CH:13]=1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 2723982Triethyloxonium tetrafluoroborateHCID 200417145,7-dihydro-6H-dibenz[c,e]azepine-6-carboxamide

생성물 1

HCID 19833914ethyl 5,7-dihydro-6H-dibenz[c,e]azepine-6carboximidate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1.19 g of 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboxamide are dissolved in 10 ml of methylene chloride, and the solution is treated with 1.14 g of triethyloxonium tetrafluoroborate and stirred at room temperature for 20 hours. The mixture is then poured on to 10% sodium carbonate solution/ice and the whole is extracted with methylene chloride. The combined extracts are washed with 10% sodium carbonate solution, dried over anhydrous sodium sulphate and evaporated under reduced pressure. In this manner there is obtained crude ethyl 5,7-dihydro-6H-dibenz[c,e]azepine-6-caboximidate which is purified by a filtration on silica gel [eluent: n-hexane/ethyl acetate (1:1)]; m.p. 74°-76° C. (crystallized from n-hexane).

후처리

  1. extractionthe whole is extracted with methylene chloride
  2. washThe combined extracts are washed with 10% sodium carbonate solution
  3. dry with materialdried over anhydrous sodium sulphate
  4. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-62a3a9f5b00e4b3493aa4800d32f3db5
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766115

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