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1H-1,2,4-Triazole → HCID 14403430, 화합물

HRID 703353
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인쇄 미리보기

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HRID 703353 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH:9]=[CH:10][C:11]1([C:14]2([S:17][CH2:18][CH2:19][CH3:20])[CH2:16][CH2:15]2)[CH2:13][O:12]1.[NH:21]1[CH:25]=[N:24][CH:23]=[N:22]1>CN(C)C=O.C(OCC)(=O)C.C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1/[CH:9]=[CH:10]/[C:11]([C:14]1([S:17][CH2:18][CH2:19][CH3:20])[CH2:16][CH2:15]1)([OH:12])[CH2:13][N:21]1[CH:25]=[N:24][CH:23]=[N:22]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 92571H-1,2,4-TriazoleHCID 540874812-(2,4-Dichlorophenylethenyl)-2-(1-propylmercaptocyclopropyl) oxirane

생성물 1

HCID 14403430HCID 14403430, 화합물수율 26%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회HCID 21584019Toluene ethylacetate용매

반응 조건

온도
80 °C

실험 절차

A solution of 38.2 g (0.12 mol) of 2-(2,4-dichlorophenyl-ethenyl)-2-(1-propylmercaptocyclopropyl)-oxirane in 30 ml of dimethylformamide is added dropwise at 80° C. under a nitrogen atmosphere and with stirring to a mixture of 24 g (0.35 mol) of 1,2,4-triazole, 2.7 g (0.02 mol) of potassium tert.-butylate and 50 ml of dimethylformamide. The mixture is stirred for 6 hours at 80° C., then the solvent is stripped off under reduced pressure, and the residue is taken up in ethyl acetate/toluene, washed using water, dried over sodium sulphate and concentrated under reduced pressure. The residue remaining is chromatographed on silica gel using chloroform as eluant. In this manner, 12.1 g (26% of theory) of trans-4-(2,4-dichlorophenyl)-2-(1-propylmercaptocyclopropyl)-1-(1,2,4-triazol-1-yl)-but-3-en-2-ol are obtained in the form of an oily product.

후처리

  1. washwashed
  2. dry with materialdried over sodium sulphate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue remaining is chromatographed on silica gel

출처 및 근거

ORD 기록
ord-558a8957b80f4948ba5fbf4d3c06b592
출처 데이터셋
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04983208

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