CID 15930840 → 5-[4-(3-Isopropyl-4-methoxy-phenoxy)-3,5-dimethyl-phenyl]-2,4-dihydro-[1,2,4]triazol-3-one

HRID 1062484

반응식

HRID 1062484 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([CH:11]=[C:12]([CH3:26])[C:13]=1[O:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[C:17]([CH:23]([CH3:25])[CH3:24])[CH:16]=1)[CH:5]=[N:6][NH:7][C:8]([NH2:10])=[O:9].[S]Cl>C(OCC)(=O)C.C(O)(=O)C>[CH:23]([C:17]1[CH:16]=[C:15]([CH:20]=[CH:19][C:18]=1[O:21][CH3:22])[O:14][C:13]1[C:2]([CH3:1])=[CH:3][C:4]([C:5]2[NH:10][C:8](=[O:9])[NH:7][N:6]=2)=[CH:11][C:12]=1[CH3:26])([CH3:24])[CH3:25]

참가 물질

4

반응물 2

HCID 15930840CID 15930840HCID 697550043,5-Dimethyl-4-(3-isopropyl-4-methoxy-phenoxy)-benzaldehyde-semicarbazone

생성물 1

HCID 1355559405-[4-(3-Isopropyl-4-methoxy-phenoxy)-3,5-dimethyl-phenyl]-2,4-dihydro-[1,2,4]triazol-3-one수율 24.2%

시약·촉매·용매 1

HCID 22609514Ethyl acetate acetate용매

실험 절차

A solution of the title compound of Step A (20 mg, 0.055 mmol) and sulfur monochloride (26.7 μl, 0.33 mmol) in ethyl acetate/acetic acid (2.4 ml/0.6 ml) was heated to reflux for about eight hours. The mixture was concentrated and the residue was purified by preparative TLC (5% methanol in dichloromethane) to afford the title compound (4.7 mg) as a white solid. MS (APCI+) Calc: 353.2, found: 354.2 (M+1).

후처리

  1. temperatureto reflux for about eight hours
  2. concentrationThe mixture was concentrated
  3. customthe residue was purified by preparative TLC (5% methanol in dichloromethane)

출처 및 근거

ORD 기록
ord-812c2fbc8a81476a9ee2deea69fe3651
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06960604B2

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