聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → HCID 22868545，化合物

HRID 232759

反应方程式

HRID 232759 反应方程式
[O:1]1[C:5]2([CH2:10][CH2:9][NH:8][CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.O.[O:12]1[C@H:14]2[CH2:15][C@H:16]3[C@:29]([CH3:31])([CH2:30][C@@H:13]12)[C@@H:28]1[C@H:19]([C@H:20]2[C@@:24]([CH2:26][CH2:27]1)([CH3:25])[C@@H:23]([OH:32])[C@@H:22]([N:33]1[CH2:37][CH2:36][CH2:35][CH2:34]1)[CH2:21]2)[CH2:18][CH2:17]3>C(#N)C>[O:1]1[C:5]2([CH2:10][CH2:9][N:8]([C@H:13]3[CH2:30][C@@:29]4([CH3:31])[C@@H:16]([CH2:17][CH2:18][C@@H:19]5[C@@H:28]4[CH2:27][CH2:26][C@@:24]4([CH3:25])[C@H:20]5[CH2:21][C@H:22]([N:33]5[CH2:37][CH2:36][CH2:35][CH2:34]5)[C@@H:23]4[OH:32])[CH2:15][C@@H:14]3[OH:12])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1

参与物

5

反应物 3

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 674354-哌啶酮缩乙二醇HCID 16063872(2α,3α,5α，16β,17β)-2,3-环氧-16-(1-吡咯烷)-雄甾烷-17-醇

产物 1

HCID 22868545HCID 22868545，化合物

试剂、催化剂与溶剂 1

HCID 6342乙腈溶剂

实验过程

After adding 63 g of 1,4-dioxa-8-azaspiro[4.5]decane and 13 ml of water to 17 g of 2α,3α-epoxy-16β-(1-pyrrolidinyl)-5α-androstane-17β-ol, the reaction mixture is maintained at 100° to 105° C. for 80 hours while introducing nitrogen. After completion of the reaction, the solution containing a precipitate is diluted with 200 ml of acetonitrile and after filtering, the precipitate is thoroughly washed with water and then with acetonitrile, dried and recrystallized from methanol to give the title product in a yield of 18.2 g (76.5%), m.p.: 184°-187° C.

后处理

  1. temperaturethe reaction mixture is maintained at 100° to 105° C. for 80 hours
  2. additionwhile introducing nitrogen
  3. customAfter completion of the reaction
  4. additionthe solution containing a precipitate
  5. filtrationafter filtering
  6. washthe precipitate is thoroughly washed with water
  7. dry with materialwith acetonitrile, dried
  8. customrecrystallized from methanol

来源与证据

ORD记录
ord-d432d9d21a9f4e12b3cc1722ac9e8480
来源数据集
uspto-grants-1997_01
专利号
US05591735

关联笔记

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