聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 二苄醚

HRID 36094

反应方程式

HRID 36094 反应方程式
C(O[CH2:9][C@@H:10]1[C@@H:13]([CH2:14][O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:12][C:11]1=O)C1C=CC=CC=1.P(O)(O)O.O.[CH:29](O)(C)C>[Ir](Cl)(Cl)(Cl)Cl>[CH2:16]([O:15][CH2:14][C:13]1[CH:10]=[CH:9][CH:29]=[CH:11][CH:12]=1)[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1

参与物

6

反应物 4

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 3776异丙醇HCID 107909正亚磷酸HCID 14863583(2S-trans)-2,3-bis[(benzyloxy)methyl]cyclobutanone

产物 1

HCID 7657二苄醚

试剂、催化剂与溶剂 1

HCID 24815四氯化铱催化剂

实验过程

A mixture of (2S-trans)-2,3-bis[(benzyloxy)methyl]cyclobutanone (0.25 g., 0.806 mmole), iridium tetrachloride (0.016 g., 0.0483 mmole), phosphorous acid (0.397 g., 4.84 mmole) and water (0.3 ml.) in isopropanol (3 ml.) was refluxed overnight. The solvent was evaporated on a rotary evaporator. The residue was taken up in ethyl acetate and washed successively with 10% hydrochloric acid, brine, and 5% sodium bicarbonate. The organic layer was dried (magnesium sulfate) and the solvent was evaporated to give [1S-(1α,2β,3β)]-3-hydroxy-1,2-cyclobutanedimethanol, dibenzyl ether; TLC (40% ethyl acetate/hexane) Rf =0.51.

后处理

  1. temperaturewas refluxed overnight
  2. customThe solvent was evaporated on a rotary evaporator
  3. washwashed successively with 10% hydrochloric acid, brine, and 5% sodium bicarbonate
  4. dry with materialThe organic layer was dried (magnesium sulfate)
  5. customthe solvent was evaporated

来源与证据

ORD记录
ord-1ee0d42dc8654c73a17e61c3bd3a2269
来源数据集
uspto-grants-1995_05
专利号
US05412134

关联笔记

加载中…