Water → (4-(3-(2-Chlorobenzoyl)-5-ethylthiophen-2-yl)-5-methyl[1,2,4]triazol-3-ylmethyl)-3,4-dichlorobenzoate

HRID 963047노트

반응식

HRID 963047 반응식
[Cl:1][C:2]1[CH:24]=[CH:23][CH:22]=[CH:21][C:3]=1[C:4]([C:6]1[CH:10]=[C:9]([CH2:11][CH3:12])[S:8][C:7]=1[N:13]1[C:17]([CH3:18])=[N:16][N:15]=[C:14]1[CH2:19][OH:20])=[O:5].C(N(CC)CC)C.[Cl:32][C:33]1[CH:34]=[C:35]([CH:39]=[CH:40][C:41]=1[Cl:42])[C:36](Cl)=[O:37].O>C(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:24]=[CH:23][CH:22]=[CH:21][C:3]=1[C:4]([C:6]1[CH:10]=[C:9]([CH2:11][CH3:12])[S:8][C:7]=1[N:13]1[C:17]([CH3:18])=[N:16][N:15]=[C:14]1[CH2:19][O:20][C:36](=[O:37])[C:35]1[CH:39]=[CH:40][C:41]([Cl:42])=[C:33]([Cl:32])[CH:34]=1)=[O:5]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 76403Benzoyl chloride, 3,4-dichloro-HCID 190851734-(3-(2-Chlorobenzoyl)-5-ethylthiophen-2-yl)-3-hydroxymethyl-5-methyl[1,2,4]triazole

생성물 1

HCID 19085140(4-(3-(2-Chlorobenzoyl)-5-ethylthiophen-2-yl)-5-methyl[1,2,4]triazol-3-ylmethyl)-3,4-dichlorobenzoate수율 68.9%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

4-(3-(2-Chlorobenzoyl)-5-ethylthiophen-2-yl)-3-hydroxymethyl-5-methyl[1,2,4]triazole (1.08 g) was dissolved in chloroform (50 ml). Triethylamine (0.34 g) and 3,4-dichlorobenzoyl chloride (0.69 g) were added, and the mixture was stirred at room temperature for 2 hours. Then, water was added to the solution for washing, and the mixture was dried over magnesium sulfate. The solvent was evaporated, and the residue was purified by silica gel column chromatography (developing solvent:ethyl acetate-methanol) and recrystallized from ethyl acetate-diisopropyl ether to give 1.10 g of (4-(3-(2-chlorobenzoyl)-5-ethylthiophen-2-yl)-5-methyl[1,2,4]triazol-3-ylmethyl)-3,4-dichlorobenzoate.

후처리

  1. washfor washing
  2. dry with materialthe mixture was dried over magnesium sulfate
  3. customThe solvent was evaporated
  4. customthe residue was purified by silica gel column chromatography (developing solvent:ethyl acetate-methanol)
  5. customrecrystallized from ethyl acetate-diisopropyl ether

출처 및 근거

ORD 기록
ord-c280b730bc7c424c959dd3b180727168
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05760032

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