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HRID128212

反应详情

EQUATION

反应方程式

HRID 128212 的结构方程式

REACTANTS

反应物

3
结构：Cl
HCID313

Hydrochloric Acid

ClH

结构：C=P(c1ccccc1)(c1ccccc1)c1ccccc1
HCID137960

Methylenetriphenylphosphorane

C19H17P

结构：COc1ccc2c(c1)[C@]13CCN(CC4CCC4)[C@H](C2)[C@@H]1[C@@H](C)CC(=O)C3
HCID56616253

未命名化合物

PRODUCTS

生成物

1
结构：C=C1C[C@H](C)[C@H]2[C@H]3Cc4ccc(OC)cc4[C@@]2(CCN3CC2CCC2)C1.Cl
HCID70527923

未命名化合物

收率 37%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CS(C)=O
溶剂HCID679

Dimethyl sulfoxide

C2H6OS

PROCEDURE

实验过程

To a solution of methylenetriphenylphosphorane (14.4 mmole) in dimethyl sulfoxide (30 ml) prepared in the usual fashion was added a solution of 17-cyclobutylmethyl-3-methoxy-8β-methyl-morphinan-6-one. The reaction was heated at 75° for 2 hours under an atmosphere of nitrogen. Workup followed by chromatography gave the free base of TR-5377 as a foam. This was converted to the HCl salt which was crystallized from toluene to give 860 mg (37%) of TR-5377, mp. 221°-224°.

WORKUP

后处理

  1. temperatureThe reaction was heated at 75° for 2 hours under an atmosphere of nitrogen
  2. customgave the free base of TR-5377 as a foam
  3. customwas crystallized from toluene