Water → HCID 22868545、化合物

HRID 232759

反応式

HRID 232759 の反応式
[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

参加物

5

反応物 3

HCID 962WaterHCID 674351,4-Dioxa-8-azaspiro(4.5)decaneHCID 160638722Alpha,3alpha-epoxy-16beta-(1-pyrrolidinyl)-5alpha-androstan-17beta-OL

生成物 1

HCID 22868545HCID 22868545、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d432d9d21a9f4e12b3cc1722ac9e8480
出典データセット
uspto-grants-1997_01
特許番号
US05591735

関連ノート

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