Hydrochloric Acid → 2-[2-chloro-4-fluoro-5-(4-difluoromethyl-4,5-dihydro-3-methyl-5-oxo-1H-1,2,4-triazol-1-yl)phenoxy]pyridine-5-diazonium tetrafluoroborate

HRID 1090984노트

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HRID 1090984 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([O:8][C:9]2[C:10]([Cl:26])=[CH:11][C:12]([F:25])=[C:13]([N:15]3[C:19](=[O:20])[N:18]([CH:21]([F:23])[F:22])[C:17]([CH3:24])=[N:16]3)[CH:14]=2)=[N:6][CH:7]=1.Cl.[N:28]([O-])=O.[Na+].[F:32][B-:33]([F:36])([F:35])[F:34].[Na+]>O>[F:32][B-:33]([F:36])([F:35])[F:34].[Cl:26][C:10]1[CH:11]=[C:12]([F:25])[C:13]([N:15]2[C:19](=[O:20])[N:18]([CH:21]([F:22])[F:23])[C:17]([CH3:24])=[N:16]2)=[CH:14][C:9]=1[O:8][C:5]1[CH:4]=[CH:3][C:2]([N+:1]#[N:28])=[CH:7][N:6]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 4343483Sodium TetrafluoroborateHCID 199122051-[5-(5-aminopyridin-2-yloxy)-4-chloro-2-fluorophenyl]-4-difluoromethyl-4,5-dihydro-3-methyl-1,2,4-triazol-5(1H)-oneHCID 23668193Sodium Nitrite

생성물 1

HCID 199122182-[2-chloro-4-fluoro-5-(4-difluoromethyl-4,5-dihydro-3-methyl-5-oxo-1H-1,2,4-triazol-1-yl)phenoxy]pyridine-5-diazonium tetrafluoroborate수율 97%

시약·촉매·용매 1

HCID 962Water용매4회

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온도
0 °C

실험 절차

To a stirred mixture of 3.9 g (0.010 mole) of 1-[5-(5-aminopyridin-2-yloxy)-4-chloro-2-fluorophenyl]-4-difluoromethyl-4,5-dihydro-3-methyl-1,2,4-triazol-5(1H)-one in 10 mL of water was added 5.0 mL of concentrated hydrochloric acid. The mixture was cooled in an ice water bath, and a solution of 0.76 g (0.011 mole) of sodium nitrite in 1.4 mL of water was added portionwise. The resultant mixture was stirred at 0° C. for 30 minutes, and a solution of 1.5 g (0.014 mole) of sodium tetrafluoroborate in 5 mL of water was added portionwise. An additional 5 mL of water was added, and the reaction mixture was stirred at 0° C. for 45 minutes. The mixture was filtered, and the filter cake was rinsed with ice water followed by diethyl ether. The filter cake was dried under reduced pressure to yield 4.7 g of 2-[2-chloro-4 -fluoro-5-(4-difluoromethyl-4,5-dihydro -3-methyl-5-oxo-1H-1,2,4-triazol-1-yl)phenoxy]pyridine-5-diazonium tetrafluoroborate.

후처리

  1. temperatureThe mixture was cooled in an ice water bath
  2. filtrationThe mixture was filtered
  3. washthe filter cake was rinsed with ice water
  4. customThe filter cake was dried under reduced pressure

출처 및 근거

ORD 기록
ord-d7948bcf10d048838df6d427ac40076c
출처 데이터셋
uspto-grants-1992_01
특허 번호
US05084085

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