p-Toluenesulfonic acid → HCID 15307268, 화합물

HRID 850825노트

반응식

HRID 850825 반응식
[OH:1][C:2]1[CH:19]=[CH:18][C:17]2[C@@H:16]3[C@H:7]([C@H:8]4[C@@:12]([CH2:14][CH2:15]3)([CH3:13])[C:11](=[O:20])[CH2:10][CH2:9]4)[CH:6]=[CH:5][C:4]=2[CH:3]=1.[C:21]1(C)C=[CH:25][C:24](S(O)(=O)=O)=[CH:23][CH:22]=1.[O:32]1CCCC1>O1C=CCCC1.C(OCC)(=O)C>[O:32]1[CH2:25][CH2:24][CH2:23][CH2:22][CH:21]1[O:1][C:2]1[CH:19]=[CH:18][C:17]2[C@@H:16]3[C@H:7]([C@H:8]4[C@@:12]([CH2:14][CH2:15]3)([CH3:13])[C:11](=[O:20])[CH2:10][CH2:9]4)[CH:6]=[CH:5][C:4]=2[CH:3]=1

참가 물질

6

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 8028TetrahydrofuranHCID 1022253-Hydroxyestra-1,3,5(10),6-tetraen-17-one

생성물 1

HCID 15307268HCID 15307268, 화합물

시약·촉매·용매 2

HCID 80803,4-dihydro-2H-pyran용매HCID 8857Ethyl Acetate용매

실험 절차

A suspension of 2.6 g of 3-hydroxy-estra-1,3,5(10),6-tetraen-17-one in 26 ml of tetrahydrofuran and 2.6 ml of dihydropyran is stirred with 12.3 mg of para-toluenesulfonic acid for 3 hours at room temperature. Then, it is diluted with ethyl acetate, washed with sodium bicarbonate solution as well as with saturated sodium chloride solution, dried on sodium sulfate and concentrated by evaporation in a vacuum. 3.0 g of 3-tetrahydropyranyloxy-estra-1,3,5(10),6-tetraen-17-one is obtained as colorless crystals.

후처리

  1. washwashed with sodium bicarbonate solution as well as with saturated sodium chloride solution
  2. customdried on sodium sulfate
  3. concentrationconcentrated by evaporation in a vacuum

출처 및 근거

ORD 기록
ord-40f88a932e9e4ee3988d32bbecbe111c
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06018062

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