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HRID222203

反应详情

EQUATION

反应方程式

HRID 222203 的结构方程式

REACTANTS

反应物

3
结构：CC(=O)O
HCID176

Acetic Acid

C2H4O2

结构：O
HCID962

Water

H2O

结构：CC(C)(C)[Si](C)(C)OC[C@@H]1C[C@@H](n2ccc3c(N[C@H]4CCc5ccccc54)ncnc32)C[C@@H]1O[Si](C)(C)C(C)(C)C
HCID58944666

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)(C)[Si](C)(C)O[C@H]1C[C@H](n2ccc3c(N[C@H]4CCc5ccccc54)ncnc32)C[C@H]1CO
HCID58944620

未命名化合物

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
40 °C

PROCEDURE

实验过程

7-[(1R,3S,4S)-3-[tert-butyl(dimethyl)silyl]oxy-4-([tert-butyl(dimethyl)silyl]-oxymethyl)cyclopentyl]-N-[(1S)-2,3-dihydro-1H-inden-1-yl]-7H-pyrrolo[2,3-d]pyrimidin-4-amine (1.66 g, 0.00280 mol) was dissolved in a mixture of tetrahydrofuran (6.6 mL), water (6.6 mL, 0.36 mol), and acetic acid (19 mL, 0.34 mol). The solution was then heated to 40° C. overnight. The mixture was then cooled and evaporated, azeotroped with toluene (2×50 mL) and the residue was purified by silica gel chromatography eluting with 0 to 100% ethyl acetate in dichloromethane to yield the product as a white solid, 1.05 g (74%). LC/MS: Rt=1.68 min, ES+ 479 (AA standard).

WORKUP

后处理

  1. temperatureThe mixture was then cooled
  2. customevaporated
  3. customazeotroped with toluene (2×50 mL)
  4. customthe residue was purified by silica gel chromatography
  5. washeluting with 0 to 100% ethyl acetate in dichloromethane