p-Toluenesulfonic acid → HCID 15307268、化合物

HRID 850825ノート

反応式

HRID 850825 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 15307268HCID 15307268、化合物

試薬・触媒・溶媒 2

HCID 80803,4-dihydro-2H-pyran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-40f88a932e9e4ee3988d32bbecbe111c
出典データセット
uspto-grants-2000_01
特許番号
US06018062

反応ノート

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