Potassium Carbonate → 3-((4-methyl-4H-1,2,4-triazol-3-yl)sulphanyl)propan-1-ol

HRID 454207노트

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HRID 454207 반응식
[CH3:1][N:2]1[CH:6]=[N:5][N:4]=[C:3]1[SH:7].Br[CH2:9][CH2:10][CH2:11][OH:12].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:1][N:2]1[CH:6]=[N:5][N:4]=[C:3]1[S:7][CH2:9][CH2:10][CH2:11][OH:12]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 123083-Bromo-1-propanolHCID 178481306HCID 178481306, 화합물

생성물 1

HCID 220306083-((4-methyl-4H-1,2,4-triazol-3-yl)sulphanyl)propan-1-ol수율 30%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
40 °C

실험 절차

A solution of 4-methyl-4-H-1,2,4-triazole-3-thiol (1.72 g, 15 mmol) and 3-bromopropan-1-ol (1.39 g, 10 mmol) in DMF (10 ml) containing potassium carbonate (1.57 g, 14 mmol) was heated at 40° C. for 30 minutes. The mixture was then partitioned between saturated ammonium chloride and ethyl acetate. The aqueous layer was evaporated to dryness and the residue was triturated with ethyl acetate and methylene chloride. The suspension was filtered and the filtrate was dried (MgSO4) and evaporated. The residue was purified by column chromatography eluting with methylene chloride/methanol (9/1) to give 3-((4-methyl-4H-1,2,4-triazol-3-yl)sulphanyl)propan-1-ol (510 mg, 30%).

후처리

  1. customThe mixture was then partitioned between saturated ammonium chloride and ethyl acetate
  2. customThe aqueous layer was evaporated to dryness
  3. customthe residue was triturated with ethyl acetate and methylene chloride
  4. filtrationThe suspension was filtered
  5. dry with materialthe filtrate was dried (MgSO4)
  6. customevaporated
  7. customThe residue was purified by column chromatography
  8. washeluting with methylene chloride/methanol (9/1)

출처 및 근거

ORD 기록
ord-d92db9b5f22e4efca70f456c2c93d6b2
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08492560B2

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