Water → HCID 68560345, 화합물

HRID 1876735노트

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HRID 1876735 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 (III) 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 free of mother liquor and dried. The 15α-acetoxy-androst-4-ene-3,7-dione is obtained with 88% yield. The reaction is easy-to-carry out, there are no safety and scale-up problems. The 15α-acetoxy compound obtained can be used in the next reaction step without purification.

후처리

  1. filtrationis filtered
  2. washwashed until free of mother liquor
  3. customdried

출처 및 근거

ORD 기록
ord-4fb3c416d0504fa7b196ed68e81c1f5e
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08309712B2

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