HRID1045072

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID176

Acetic Acid

C2H4O2

HCID11430

Potassium Carbonate

CK2O3

结构：CCCSc1nc(Cl)c(N)c(N[C@@H]2C[C@H](OCCO)[C@H]3OC(C)(C)O[C@H]32)n1

HCID10202186

2-[[(3aR,4S,6R,6aS)-6-[[5-Amino-6-chloro-2-(propylthio)-4-pyrimidinyl]amino]tetrahydro-2,2-dimethyl-4H-cyclopenta-1,3-dioxol-4-yl]oxy]ethanol

C17H27ClN4O4S

HCID23668193

Sodium Nitrite

NNaO2

PRODUCTS

生成物

结构：CCCSc1nc(Cl)c2nnn([C@@H]3C[C@H](OCCO)[C@H]4OC(C)(C)O[C@H]43)c2n1

HCID21035774

2-[[(3aR,4S,6R,6aS)-6-[7-Chloro-5-(propylthio)-3H-1,2,3-triazolo[4,5-d]pyrimidin-3-yl]tetrahydro-2,2-dimethyl-4H-cyclopenta-1,3-dioxol-4-yl]oxy]ethanol

C17H24ClN5O4S

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID962

Water

H2O

2 次

溶剂HCID1140

Toluene

C7H8

PROCEDURE

实验过程

2-[((3aR,4S,6R,6aS)-6-{[5-Amino-6-chloro-2-(propylthio)pyrimidin-4-yl]amino}-2,2-dimethyl-tetrahydro-3aH-cyclopenta[d][1,3]dioxol-4-yl)oxy]ethanol (320 kg) and sodium nitrite (61 kg) were dissolved in a mixture of water (224 kg) and toluene (1450 kg) at room temperature. Acetic acid (276 kg) was charged with a rate that kept the temperature of the reaction ≦30° C. After full conversion was reached (≧99.9%), potassium carbonate (317 kg) dissolved in water (640 kg) was added to the reaction solution. After the extraction the water layer was separated off and the organic layer was used in the next step.

WORKUP

后处理

customthe temperature of the reaction ≦30° C
additionwas added to the reaction solution
extractionAfter the extraction the water layer
customwas separated off