聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → [2-(Trifluoromethyl)-1H-indol-3-yl]methanol

HRID 231836

反应方程式

HRID 231836 反应方程式
[BH4-].[K+].[F:3][C:4]([F:17])([F:16])[C:5]1[NH:6][C:7]2[C:12]([C:13]=1[CH:14]=[O:15])=[CH:11][CH:10]=[CH:9][CH:8]=2.O1CCCC1.O>CCOCC>[F:17][C:4]([F:3])([F:16])[C:5]1[NH:6][C:7]2[C:12]([C:13]=1[CH2:14][OH:15])=[CH:11][CH:10]=[CH:9][CH:8]=2

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 8028四氢呋喃2 次HCID 4192641硼氢化钾HCID 200321282-trifluoromethyl-3-formyl-(1H)-indole

产物 1

HCID 20032113[2-(Trifluoromethyl)-1H-indol-3-yl]methanol收率 64.6%

试剂、催化剂与溶剂 1

HCID 3283乙醚溶剂

实验过程

2 g of potassium borohydride were added in small fractions at +5° C. to a solution of 4.6 g of the product of Step A, 150 ml of tetrahydrofuran and 30 ml of water and the mixture was stirred for one hour. The mixture was allowed to return to ambient temperature and the tetrahydrofuran was eliminated under reduced pressure. The resulting mixture was diluted with ether, washed with water, dried and concentrated under reduced pressure. The residue was chromatographed over silica (eluent: hexaneethyl acetate 7-3) to obtain 3 g of 2-trifluoromethyl-(1H)-indol-3-yl methanol melting at 106° C.

后处理

  1. customto return to ambient temperature
  2. washwashed with water
  3. customdried
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was chromatographed over silica (eluent: hexaneethyl acetate 7-3)

来源与证据

ORD记录
ord-ad967951fb5a48f7bfe9f3319054f3fa
来源数据集
uspto-grants-1989_07
专利号
US04849443

关联笔记

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