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HRID1045071

反应详情

EQUATION

反应方程式

HRID 1045071 的结构方程式

REACTANTS

反应物

4
结构：CC(=O)O
HCID176

Acetic Acid

C2H4O2

结构：O=C([O-])[O-].[K+].[K+]
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

结构：O=N[O-].[Na+]
HCID23668193

Sodium Nitrite

NNaO2

PRODUCTS

生成物

1
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

2
结构：O
溶剂HCID962

Water

H2O

3 次

结构：Cc1ccccc1
溶剂HCID1140

Toluene

C7H8

PROCEDURE

实验过程

To 2-[((3 aR,4S,6R,6aS)-6-{[5-Amino-6-chloro-2-(propylthio)pyrimidin-4-yl]amino}-2,2-dimethyltetrahydro-3 aH-cyclopenta[d][1,3]dioxol-4-yl)oxy]ethanol (180 kg) in toluene (749 kg) and acetic acid (153 kg) were added sodium nitrite (33.2 kg) in water (88 kg) charged with a rate that kept the temperature of the reaction ≦30° C. After the conversion criterion was reached (>99%) potassium carbonate (176 kg) in water (360 kg) was added to the reaction solution whereafter the water layer was separated off and the organic-layer was used in the next step.

WORKUP

后处理

  1. additioncharged with a rate that
  2. customthe temperature of the reaction ≦30° C
  3. customwas separated off