Methanol → 5-(5-(3-chloropropylthio)-4-methyl-4H-1,2,4-triazol-3-yl)-2,4-dimethylthiazole

HRID 1661064노트

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HRID 1661064 반응식
[CH3:1][C:2]1[S:3][C:4]([C:8]2[N:9]([CH3:14])[C:10]([SH:13])=[N:11][N:12]=2)=[C:5]([CH3:7])[N:6]=1.CO.C([O-])([O-])=O.[K+].[K+].Br[CH2:24][CH2:25][CH2:26][Cl:27]>C(OCC)(=O)C.CC(C)=O>[Cl:27][CH2:26][CH2:25][CH2:24][S:13][C:10]1[N:9]([CH3:14])[C:8]([C:4]2[S:3][C:2]([CH3:1])=[N:6][C:5]=2[CH3:7])=[N:12][N:11]=1

참가 물질

7

반응물 4

HCID 887MethanolHCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 178432727HCID 178432727, 화합물

생성물 1

HCID 446278985-(5-(3-chloropropylthio)-4-methyl-4H-1,2,4-triazol-3-yl)-2,4-dimethylthiazole수율 37.5%

시약·촉매·용매 2

HCID 180Acetone용매HCID 8857Ethyl Acetate용매

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온도
22 °C

실험 절차

5-(2,4-dimethylthiazol-5-yl)-4-methyl-4H-1,2,4-triazole-3-thiol (Prep27, 5 g, 22 mmol) was added to a mixture of methanol (15 ml) and acetone (35 ml), followed by K2CO3 (5 g, 36 mmol) and 1-bromo-3-chloropropane (35 ml, 36 mmol). The suspension was stirred at 22° C. for 24 h. The volume of solvent was reduced, then ethyl acetate (63 ml) was added and the organic layer was washed with water, the EA was removed under vacuum and the crude purified by FC (EA/MeOH 15:1) to afford 2.5 g of pure product (y=37%).

후처리

  1. washthe organic layer was washed with water
  2. customthe EA was removed under vacuum
  3. customthe crude purified by FC (EA/MeOH 15:1)

출처 및 근거

ORD 기록
ord-10eff361006c4b3ea2b609b2d6ddd6a3
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08030322B2

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