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HRID516129

反应详情

EQUATION

反应方程式

HRID 516129 的结构方程式

REACTANTS

反应物

2
结构：CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[c]1cccs1
HCID2779373

2-(Tributylstannyl)thiophene

C16H30SSn

结构：CC(C)(C)OC(=O)N[C@H]1COCC[C@H]1Nc1nc(Cl)c2c(c1F)CN(C(=O)OC(C)(C)C)C2=O
HCID86654748

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)(C)OC(=O)N[C@H]1COCC[C@H]1Nc1nc(-c2cccs2)c2c(c1F)CN(C(=O)OC(C)(C)C)C2=O
HCID67238287

未命名化合物

收率 55%

AUXILIARIES

试剂、催化剂与溶剂

3
结构：c1ccc([P](c2ccccc2)(c2ccccc2)[Pd]([P](c2ccccc2)(c2ccccc2)c2ccccc2)([P](c2ccccc2)(c2ccccc2)c2ccccc2)[P](c2ccccc2)(c2ccccc2)c2ccccc2)cc1
催化剂HCID178418397

未命名化合物

结构：Cc1ccccc1
溶剂HCID1140

Toluene

C7H8

结构：CO.ClCCl
溶剂HCID21226129

未命名化合物

PROCEDURE

实验过程

A solution of tert-butyl 6-((3R,4R)-3-(tert-butoxycarbonylamino)tetrahydro-2H-pyran-4-ylamino)-4-chloro-7-fluoro-3-oxo-1H-pyrrolo[3,4-c]pyridine-2(3H)-carboxylate (50 mg, 0.1 mmol), tributyl(thiophen-2-yl)stannane (44.7 mg, 0.12 mmol) and tetrakis(triphenylphosphine)palladium(0) (115 mg, 0.1 mmol) in toluene (3 mL) was heated to 102° C. for 24 h. The solid was filtered though a pad of Celite, and resulting crude material was reconstituted in MeOH/DCM (20 mL) and purified via preparative HPLC. The collected fractions were combined and stripped to dryness via rotary evaporation to yield the title compound (30 mg, 55%).

WORKUP

后处理

  1. filtrationThe solid was filtered though a pad of Celite
  2. customresulting crude material
  3. custompurified via preparative HPLC
  4. customstripped to dryness via rotary evaporation