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Methanol → HCID 16657482, 화합물

HRID 746202
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HRID 746202 반응식
CO.C(=O)([O-])[O-].[K+].[K+].C([O:12][CH2:13][C:14](=[O:35])[C@@H:15]1[C@:32]2([CH3:33])[C@H:18]([C@H:19]3[C@H:29]([CH2:30][CH2:31]2)[C@:27]2([CH3:28])[C:22](=[CH:23][C:24](=[O:34])[CH2:25][CH2:26]2)[CH:21]=[CH:20]3)[CH2:17][CH2:16]1)(=O)C.[CH3:36][C:37]([SH:39])=[O:38]>C(Cl)Cl>[C:37]([S:39][C@@H:20]1[CH2:21][C:22]2[C@:27]([CH3:28])([CH2:26][CH2:25][C:24](=[O:34])[CH:23]=2)[C@@H:29]2[C@@H:19]1[C@H:18]1[C@:32]([CH3:33])([CH2:31][CH2:30]2)[C@@H:15]([C:14](=[O:35])[CH2:13][OH:12])[CH2:16][CH2:17]1)(=[O:38])[CH3:36]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887MethanolHCID 10484Thioacetic acidHCID 11430Potassium CarbonateHCID 30807246-Dehydrodeoxycorticosterone acetate

생성물 1

HCID 16657482HCID 16657482, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The product of Example 3 was hydrolyzed by treating 0.5 g of the 21-acetoxy derivative in 8 ml methylene chloride with 10 ml methanol and 4 ml 0.2M aqueous potassium carbonate at room temperature under nitrogen for 30 minutes. The hydrolyzed product was extracted with methylene chloride, washed with water, dried and evaporated. A sample obtained by preparative high performance liquid chromatography showed M+ =404 daltons. An identical product was obtained by a different synthetic route involving alkaline hydrolysis of 21-acetoxy-4,6-pregnadiene-3,20-dione to the C-21-alcohol, followed by reaction with ethanethiolic acid.

후처리

  1. extractionThe hydrolyzed product was extracted with methylene chloride
  2. washwashed with water
  3. customdried
  4. customevaporated
  5. customA sample obtained by preparative high performance liquid chromatography
  6. customAn identical product was obtained by a different synthetic route

출처 및 근거

ORD 기록
ord-680aeeb5c20f494cbe5d0e2bf869ed3a
출처 데이터셋
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04603128

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