Hydrochloric Acid → HCID 67684261, 화합물

HRID 232762

반응식

HRID 232762 반응식
Cl.O1[C:6]2([CH2:11][CH2:10][N:9]([C@H:12]3[CH2:29][C@@:28]4([CH3:30])[C@@H:15]([CH2:16][CH2:17][C@@H:18]5[C@@H:27]4[CH2:26][CH2:25][C@@:23]4([CH3:24])[C@H:19]5[CH2:20][C@H:21]([N:32]5[CH2:36][CH2:35][CH2:34][CH2:33]5)[C@@H:22]4[OH:31])[CH2:14][C@@H:13]3[OH:37])[CH2:8][CH2:7]2)[O:5]CC1.[OH-].[Na+]>O1CCOCC1>[O:5]=[C:6]1[CH2:11][CH2:10][N:9]([C@H:12]2[CH2:29][C@@:28]3([CH3:30])[C@@H:15]([CH2:16][CH2:17][C@@H:18]4[C@@H:27]3[CH2:26][CH2:25][C@@:23]3([CH3:24])[C@H:19]4[CH2:20][C@H:21]([N:32]4[CH2:36][CH2:35][CH2:34][CH2:33]4)[C@@H:22]3[OH:31])[CH2:14][C@@H:13]2[OH:37])[CH2:8][CH2:7]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 228685452beta-(1,4-Dioxa-8-azaspiro[4.5]dec-8-yl)-16beta-(1-pyrrolidinyl)-5alpha-androstane-3alpha,17beta-diol

생성물 1

HCID 67684261HCID 67684261, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

After adding 42 ml of 10% aqueous hydrochloric acid solution to 5 g of 2β-(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)-16β-(1-pyrrolidinyl)-5α-androstane-3α,17β-diol dissolved in 100 ml of dioxane, the reaction mixture is boiled under reflux for 3 hours. After completion of the reaction, the solution is made alkaline by adding aqueous sodium hydroxide solution, dioxane is distilled off and the residue is diluted with water. After filtering, the precipitate is washed with water until neutral and dried. The crude product is dissolved in acetonitrile, clarified by activated carbon and after filtering off the adsorbent, two thirds of acetonitrile are distilled off. After filtering, the crystalline precipitate is dried to give the title product in a yield of 4.2 g (92.1%), m.p.: 136°-138° C.

후처리

  1. temperatureunder reflux for 3 hours
  2. customAfter completion of the reaction
  3. distillationis distilled off
  4. additionthe residue is diluted with water
  5. filtrationAfter filtering
  6. washthe precipitate is washed with water until neutral and
  7. customdried
  8. dissolutionThe crude product is dissolved in acetonitrile
  9. filtrationafter filtering off the adsorbent, two thirds of acetonitrile
  10. distillationare distilled off
  11. filtrationAfter filtering
  12. customthe crystalline precipitate is dried

출처 및 근거

ORD 기록
ord-c48eb3005e4147b0a0f93086501fc686
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05591735

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