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HRID344773

反应详情

EQUATION

反应方程式

HRID 344773 的结构方程式

REACTANTS

反应物

2
结构：CSC(=NC#N)SC
HCID66289

Dimethyl cyanocarbonodithioimidate

C4H6N2S2

结构：CC1(C)Oc2ccc(C#N)cc2[C@@H](NCCN)[C@@H]1O
HCID15680853

未命名化合物

PRODUCTS

生成物

1
结构：CC1(C)Oc2ccc(C#N)cc2[C@@H](N2CCNC2=NC#N)[C@@H]1O
HCID178431170

未命名化合物

收率 98.1%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：Cc1ccccc1
溶剂HCID1140

Toluene

C7H8

PROCEDURE

实验过程

A mixture of trans-4-(2-aminoethylamino)-6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran-3-ol (D3) (0.39g) and dimethyl N-cyanodithioiminocarbonate (0.158g) was heated under reflux in toluene (30 ml) for 71 h. The solvent was evaporated in vacuo, and the residue column chromatographed (Kieselgel 60, gradient elution: 2-7% methanol-chloroform) giving the title compound as a white solid (0.33g). Recrystallisation from ethyl acetate-ether gave a sample of m.p. 257°-260° C.

WORKUP

后处理

  1. temperaturewas heated
  2. customThe solvent was evaporated in vacuo
  3. customthe residue column chromatographed
  4. wash(Kieselgel 60, gradient elution: 2-7% methanol-chloroform)