Diethyl Carbonate → HCID 908572, 화합물

HRID 1979717노트

반응식

HRID 1979717 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9](=[CH:15][C:16](=[O:18])[NH2:17])[NH:8][CH2:7][CH2:6]2.[O-:19][CH2:20]C.[Na+].C(=O)(OCC)OCC>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9]1=[CH:15][C:16](=[O:18])[NH:17][C:20](=[O:19])[N:8]1[CH2:7][CH2:6]2

참가 물질

5

반응물 3

HCID 7766Diethyl CarbonateHCID 2723922Sodium ethoxideHCID 704697252-(6,7-Dimethoxy-3,4-dihydroisoquinolin-1(2H)-ylidene)acetamide

생성물 1

HCID 908572HCID 908572, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 6,7-dimethoxy-1-carbamoylmethylene-1,2,3,4-tetrahydroisoquinoline (5.0g) and an excess of sodium ethoxide (prepared from 12.0 g of sodium metal and 600 ml of ethanol) in ethanol is heated. 150.0 ml of diethyl carbonate is added to the solution. The reaction mixture is refluxed for an additional 2.5 hr. The solvent is removed under vacuum and the residue is acidified to give a white precipitate, yield 4.80 g. The product crystallizes from dimethylformamide, mp. 323°-325° C.

후처리

  1. temperatureThe reaction mixture is refluxed for an additional 2.5 hr
  2. customThe solvent is removed under vacuum
  3. customto give a white precipitate, yield 4.80 g
  4. customThe product crystallizes from dimethylformamide, mp. 323°-325° C.

출처 및 근거

ORD 기록
ord-b7297953431d411e833d31b7237be5a5
출처 데이터셋
uspto-grants-1984_11
특허 번호
US04482556

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