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2-Butanethiol → HCID 178456540, 화합물

HRID 373231
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HRID 373231 반응식
[Cl:1][C:2]1[C:3](=[O:50])[N:4]([CH2:47][CH2:48][CH3:49])[C:5](=[O:46])[N:6]([CH2:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[C:22]3[N:26](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[N:25]=[N:24][N:23]=3)=[CH:12][CH:11]=2)[C:7]=1Cl.[CH:51]([SH:55])([CH2:53][CH3:54])[CH3:52].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:1][C:2]1[C:3](=[O:50])[N:4]([CH2:47][CH2:48][CH3:49])[C:5](=[O:46])[N:6]([CH2:9][C:10]2[CH:11]=[CH:12][C:13]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[C:22]3[NH:26][N:25]=[N:24][N:23]=3)=[CH:14][CH:15]=2)[C:7]=1[S:55][CH:51]([CH3:52])[CH2:53][CH3:54]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 105602-ButanethiolHCID 11430Potassium CarbonateHCID 19811540HCID 19811540, 화합물

생성물 1

HCID 178456540HCID 178456540, 화합물수율 56%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 5,6-dichloro-3-propyl-1-[[2'-(N-trityltetrazol-5-yl)biphenyl-4-yl]methyl]pyrimidine-2,4(1H,3H)-dione (0.22 g), sec-butylmercaptan (0.04 g) and potassium carbonate (0.09 g) in acetonitrile (5 ml) was heated under reflux for 4 hours. The reaction mixture was concentrated to dryness. The resulting residue was dissolved in methanol (15 ml) and 1N hydrochloric acid (1.5 ml) and the mixture was stirred at room temperature for 1 hour. The reaction mixture was concentrated to dryness and then the residue was extracted with methylene chloride-water. The organic layer was washed with water, dried, and evaporated to dryness. The resulting residue was purified by column chromatography on silica gel to give yellow amorphous powders (90 mg, 56%).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 4 hours
  3. concentrationThe reaction mixture was concentrated to dryness
  4. dissolutionThe resulting residue was dissolved in methanol (15 ml)
  5. concentrationThe reaction mixture was concentrated to dryness
  6. extractionthe residue was extracted with methylene chloride-water
  7. washThe organic layer was washed with water
  8. customdried
  9. customevaporated to dryness
  10. customThe resulting residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-c8ea2189ee6b4b61903cdd22a0f5e1ca
출처 데이터셋
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05162326

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