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Lithium Hydroxide → 5-difluoromethyl-2-methyl-4-(2-methyl-5-phenylbenzyl)-2,4-dihydro-3H-1,2,4-triazol-3-one

HRID 1883628
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HRID 1883628 반응식
[F:1][CH:2]([F:10])[C:3]1[NH:4][C:5](=[O:9])[N:6]([CH3:8])[N:7]=1.[OH-].[Li+].[I-].[Na+].[CH3:15][C:16]1[CH:23]=[CH:22][C:21]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[CH:20][C:17]=1[CH2:18]Cl>C1(C)C=CC=CC=1>[F:1][CH:2]([F:10])[C:3]1[N:4]([CH2:18][C:17]2[CH:20]=[C:21]([C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=3)[CH:22]=[CH:23][C:16]=2[CH3:15])[C:5](=[O:9])[N:6]([CH3:8])[N:7]=1.[F:1][CH:2]([F:10])[C:3]1[N:4]=[C:5]([O:9][CH2:18][C:17]2[CH:20]=[C:21]([C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=3)[CH:22]=[CH:23][C:16]=2[CH3:15])[N:6]([CH3:8])[N:7]=1
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참가 물질

7

반응물 4

HCID 3939Lithium HydroxideHCID 5238Sodium IodideHCID 235082292-Methyl-5-phenylbenzyl chlorideHCID 1358382515-(Difluoromethyl)-2-methyl-1H-1,2,4-triazol-3(2H)-one

생성물 2

HCID 120565215-difluoromethyl-2-methyl-4-(2-methyl-5-phenylbenzyl)-2,4-dihydro-3H-1,2,4-triazol-3-one
HCID 23508214
3-difluoromethyl-1-methyl-5-(2-methyl-5-phenylbenzyloxy)-1H-1,2,4-triazole

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixed suspension of 69 mg (0.461 mmol) of 5-difluoromethyl-2-methyl-2,4-dihydro-3H-1,2,4-triazol-3-one (produced in the same manner as in Intermediate Production Example), 12 mg (0.508 mmol) of lithium hydroxide, 14 mg (0.092 mmol) of sodium iodide and 3 ml of toluene was stirred for 2 hours while heating under reflux. Toluene was distilled off under reduced pressure, 3 ml of anhydrous 1,4-dioxane was added to the residue under nitrogen atmosphere, then, 100 mg (0.461 mmol) of 2-methyl-5-phenylbenzyl chloride was added. The reaction solution was stirred for 18 hours while heating under reflux, then, concentrated. Ethyl acetate was added to the residue, the mixture was washed with water, then, washed with saturated saline, and dried over anhydrous magnesium sulfate, then, concentrated. The residue was subjected to silica gel thin layer chromatography (eluant: hexane/ethyl acetate=3/1 (v/v)), to obtain 61 mg of 5-difluoromethyl-2-methyl-4-(2-methyl-5-phenylbenzyl)-2,4-dihydro-3H-1,2,4-triazol-3-one (Compound 1) and 11 mg of 3-difluoromethyl-1-methyl-5-(2-methyl-5-phenylbenzyloxy)-1H-1,2,4-triazole as a by-product.

후처리

  1. temperaturewhile heating
  2. temperatureunder reflux
  3. distillationToluene was distilled off under reduced pressure, 3 ml of anhydrous 1,4-dioxane
  4. additionwas added to the residue under nitrogen atmosphere
  5. stirringThe reaction solution was stirred for 18 hours
  6. temperaturewhile heating
  7. temperatureunder reflux
  8. concentrationconcentrated
  9. additionEthyl acetate was added to the residue
  10. washthe mixture was washed with water
  11. washwashed with saturated saline
  12. dry with materialdried over anhydrous magnesium sulfate
  13. concentrationconcentrated

출처 및 근거

ORD 기록
ord-7914c2f9fc804d65bfc0b314e8603f6c
출처 데이터셋
uspto-grants-2004_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06762197B2

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