Chlorodifluoromethane → 4-Difluoromethyl-3-methyl-1-phenyl-1H-1,2,4-triazol-5(4H)-one

HRID 1292488

반응식

HRID 1292488 반응식
[CH3:1][C:2]1[NH:6][C:5](=[O:7])[N:4]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:3]=1.[OH-].[Na+].C(=O)([O-])[O-].[K+].[K+].Cl[CH:23]([F:25])[F:24]>O.COCCOCCOCCOCCOC>[F:24][CH:23]([F:25])[N:6]1[C:5](=[O:7])[N:4]([C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:3]=[C:2]1[CH3:1]

참가 물질

7

반응물 4

HCID 6372ChlorodifluoromethaneHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 1355376213-Methyl-1-phenyl-4,5-dihydro-1H-1,2,4-triazol-5-one

생성물 1

HCID 110854614-Difluoromethyl-3-methyl-1-phenyl-1H-1,2,4-triazol-5(4H)-one수율 98.3%

시약·촉매·용매 2

HCID 962Water용매HCID 8925Tetraglyme용매

실험 절차

This compound was prepared in the manner of Example 3, with 50.0 grams of 4,5-dihydro-3-methyl-5-oxo-1-phenyl-1H-1,2,4-triazole (0.286 mole--1.0 equiv.), 11.4 grams (0.286 mole--1.0 equiv.) of sodium hydroxide in 50 mL of water, 9.9 grams (0.071 mole--0.25 equiv.) of potassium carbonate, and 37.1 grams (0.429 mole--1.5 equiv.) of chlorodifluoromethane in 333 mL of tetraglyme (% wt/vol. triazole to solvent--15%) as reagents. A yield of 63.2 grams of 96.3% pure 4-difluoromethyl-4,5-dihydro-3-methyl-5-oxo-1-phenyl-1H-1,2,4-triazole (96.6% yield) was obtained. GC analysis of the product indicated the presence of about 0.9% O-isomer by-product.

출처 및 근거

ORD 기록
ord-b54cc0cc35f244c6be0b12dd03d8794b
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05756755

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