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HRID406947

反应详情

EQUATION

反应方程式

HRID 406947 的结构方程式

REACTANTS

反应物

2
结构：O=S(=O)(O)CCS(=O)(=O)O
HCID8032

1,2-Ethanedisulfonic acid

C2H6O6S2

结构：CCOc1cc2c(cc1OC)C(c1ccc(OC)nc1OC)=N[C@@H]1CC[C@@H](O)C[C@H]21
HCID11258441

未命名化合物

PRODUCTS

生成物

1
结构：CCOc1cc2c(cc1OC)C(c1ccc(OC)nc1OC)=N[C@@H]1CC[C@@H](O)C[C@H]21.O=S(=O)(O)CCS(=O)(=O)O
HCID11855285

未命名化合物

收率 77.2%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

(2R,4aR,10bR)-6-(2,6-Dimethoxy-pyridin-3-yl)-9-ethoxy-8-methoxy-1,2,3,4,4a,10b-hexahydro-phenanthridin-2-ol (1.2 g; 2.9 mmol) is dissolved in 8.2 ml of tetrahydrofuran. The solution is heated up to 50° C. 580 mg (3.05 mmol) of ethandisulfonic acid are added. After crystallisation 1 ml ethanol is added and the suspension is stirred over night. The crystals are filtered off and dried to obtain 1.35 g (77%) of the title compound (m.p.: 233° C.).

WORKUP

后处理

  1. customAfter crystallisation 1 ml ethanol
  2. additionis added
  3. filtrationThe crystals are filtered off
  4. customdried