Water → HCID 70046759, 화합물

HRID 233642노트

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HRID 233642 반응식
S(O[CH2:12][CH2:13][O:14][C@H:15]1[CH2:32][CH2:31][C@@:30]2([CH3:33])[C@H:17]([CH2:18][CH2:19][C@@H:20]3[C@@H:29]2[CH2:28][CH2:27][C@@:25]2([CH3:26])[C@:21]3([OH:39])[CH2:22][CH2:23][C@@H:24]2[C:34]2[CH:38]=[CH:37][O:36][CH:35]=2)[CH2:16]1)(C1C=CC(C)=CC=1)(=O)=O.[NH2:40][CH2:41][CH2:42][N:43]1[CH2:47][CH2:46][CH2:45][CH2:44]1.O>C(O)C>[N:43]1([CH2:42][CH2:41][NH:40][CH2:12][CH2:13][O:14][C@H:15]2[CH2:32][CH2:31][C@@:30]3([CH3:33])[C@H:17]([CH2:18][CH2:19][C@@H:20]4[C@@H:29]3[CH2:28][CH2:27][C@@:25]3([CH3:26])[C@:21]4([OH:39])[CH2:22][CH2:23][C@@H:24]3[C:34]3[CH:38]=[CH:37][O:36][CH:35]=3)[CH2:16]2)[CH2:47][CH2:46][CH2:45][CH2:44]1

참가 물질

5

반응물 3

HCID 962WaterHCID 13441-PyrrolidineethanamineHCID 86748784HCID 86748784, 화합물

생성물 1

HCID 70046759HCID 70046759, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 0.20 g of 3β-(2-tosyloxyethoxy)-17β-(3-furyl)-5β-androstan-14β-ol in 2 ml of absolute ethanol 0.15 g of 1-(2-aminoethyl)pyrrolidine were added. The solution was kept at reflux under nitrogen for 3 hrs, then 10 ml of water were added. The residue was extracted with methylene chloride, the organic layer was washed with water to neutral pH, dried over anhydrous sodium sulfate and evaporated to dryness under reduced pressure. The crude residue was purified by flash-chromatography (SiO2) using methylene chloride/methanol 95/5 as eluant to give 0.15 g of the title compound (I-ag).

후처리

  1. temperatureat reflux under nitrogen for 3 hrs
  2. extractionThe residue was extracted with methylene chloride
  3. washthe organic layer was washed with water to neutral pH
  4. dry with materialdried over anhydrous sodium sulfate
  5. customevaporated to dryness under reduced pressure
  6. customThe crude residue was purified by flash-chromatography (SiO2)

출처 및 근거

ORD 기록
ord-026ec42c4489415184006bf6320a3b3c
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05593982

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