Diethyl Carbonate → HCID 908572、化合物

HRID 745301ノート

反応式

HRID 745301 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 908572HCID 908572、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 6,7-dimethoxy-1-carbamoylmethylene-1,2,3,4-tetrahydroisoquinoline (5.0 g) 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.

後処理

  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.

出典と根拠

ORDレコード
ord-f4de5f0e38ed4bb1a6e1f1894e99435c
出典データセット
uspto-grants-1986_07
特許番号
US04598148

反応ノート

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