Water → 2beta-(1,4-Dioxa-8-azaspiro[4.5]dec-8-yl)-16beta-(1-pyrrolidinyl)-5alpha-androstane-3alpha,17beta-diol

HRID 232759

반응식

HRID 232759 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 228685452beta-(1,4-Dioxa-8-azaspiro[4.5]dec-8-yl)-16beta-(1-pyrrolidinyl)-5alpha-androstane-3alpha,17beta-diol

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d432d9d21a9f4e12b3cc1722ac9e8480
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05591735

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