Water → HCID 68560345, 화합물

HRID 2098263노트

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HRID 2098263 반응식
[OH:1][C@@H:2]1[C@H:7]2[C@H:8]3[C@H:18]([CH2:19][CH2:20][C@:5]2([CH3:6])[C:4](=O)[CH2:3]1)[C@:16]1([CH3:17])[C:11](=[CH:12][C:13](=[O:21])[CH2:14][CH2:15]1)[CH2:10][CH2:9]3.[C:23](OC(=O)C)(=[O:25])[CH3:24].[OH2:30]>O1CCCC1.CN(C)C1C=CN=CC=1>[C:23]([O:1][C@@H:2]1[C@H:7]2[C@H:8]3[C@H:18]([CH2:19][CH2:20][C@:5]2([CH3:6])[CH2:4][CH2:3]1)[C@:16]1([CH3:17])[C:11](=[CH:12][C:13](=[O:21])[CH2:14][CH2:15]1)[CH2:10][C:9]3=[O:30])(=[O:25])[CH3:24]

참가 물질

6

반응물 3

HCID 962WaterHCID 7918Acetic AnhydrideHCID 1165238315alpha-Hydroxyandrost-4-ene-3,17-dione

생성물 1

HCID 68560345HCID 68560345, 화합물수율 88%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 8028Tetrahydrofuran용매

실험 절차

According to this invention the 15α-hydroxy-androst-4-ene-3,17-dione of the formula (II) (Chem. Ind. 1956, 111) preferably is reacted with acetic anhydride in dry tetrahydrofuran in the presence of 4-dimethylaminopyridine below a temperature of 40° C., after the reaction has been completed the reaction mixture is added to water, when the precipitate is dense enough it is filtered, washed until it is free of mother liquor and dried. The 15α-acetoxyandrost-4-ene-3,7-dione of the formula (III) is obtained with 88% yield in a process which is easy to carry out and easy to scale up to any reasonable size. The compound obtained can be used in the next reaction step without further purification.

후처리

  1. filtrationis filtered
  2. washwashed until it
  3. customdried

출처 및 근거

ORD 기록
ord-6c185f86e6f340669fd349f8549b8641
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08450476B2

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