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HRID1837266

反应详情

EQUATION

反应方程式

HRID 1837266 的结构方程式

REACTANTS

反应物

3
结构：[Cl-].[Na+]
HCID5234

Sodium chloride

ClNa

结构：CNCCCOc1ccccc1
HCID22067856

N-Methyl-3-phenoxypropan-1-amine

C10H15NO

结构：C[C@]12C[C@H](F)[C@@H]3c4ccc(O)cc4C[C@@H](CCCCCI)[C@H]3[C@@H]1CC[C@@H]2O
HCID69918427

未命名化合物

PRODUCTS

生成物

1
结构：CN(CCCCC[C@@H]1Cc2cc(O)ccc2[C@@H]2[C@@H]1[C@@H]1CC[C@H](O)[C@@]1(C)C[C@@H]2F)CCCOc1ccccc1
HCID69916332

未命名化合物

收率 84.7%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CN1CCCC1=O
溶剂HCID13387

N-Methyl-2-pyrrolidone

C5H9NO

PROCEDURE

实验过程

A solution of 486 mg of 11β-fluor-7α-(5-iodopentyl)-estra-1,3,5(10)-triene-3,17β-diol in 10 ml of 1-methyl-2-pyrrolidinone is stirred with 600 mg of methyl-(3-phenoxy-propyl)-amine for 3 hours at a bath temperature of 80° C. Then, the batch is added to saturated sodium chloride solution, extracted with ether, dried on sodium sulfate, concentrated by evaporation in a vacuum and chromatographed on silica gel with methylene chloride/methanol/ammonia. 443 mg of 11β-fluoro-7α-{5-[methyl-(3-phenoxy-propyl)-amino]-pentyl}-estra-1,3,5(10)-triene-3,17β-diol is obtained as a foam [α]D=+47° (c=0.5 in CHCl3).

WORKUP

后处理

  1. extractionextracted with ether
  2. customdried on sodium sulfate
  3. concentrationconcentrated by evaporation in a vacuum
  4. customchromatographed on silica gel with methylene chloride/methanol/ammonia