Water → 2-(4-Chloro-2-fluoro-5-hydroxyphenyl)-4-methyl-5-(trifluoromethyl)-3(2H)-pyridazinone

HRID 376822노트

반응식

HRID 376822 반응식
[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9]C(C)C)=[CH:4][C:3]=1[N:13]1[C:18](=[O:19])[C:17]([CH3:20])=[C:16]([C:21]([F:24])([F:23])[F:22])[CH:15]=[N:14]1.O>S(=O)(=O)(O)O>[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([OH:9])=[CH:4][C:3]=1[N:13]1[C:18](=[O:19])[C:17]([CH3:20])=[C:16]([C:21]([F:23])([F:24])[F:22])[CH:15]=[N:14]1

참가 물질

4

반응물 2

HCID 962WaterHCID 110898282-(2-Fluoro-4-chloro-5-isopropoxyphenyl)-4-methyl-5-trifluoromethylpyridazin-3-one

생성물 1

HCID 99490912-(4-Chloro-2-fluoro-5-hydroxyphenyl)-4-methyl-5-(trifluoromethyl)-3(2H)-pyridazinone수율 102.1%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

Then, 3.5 g (9.7 mmol) of 2-[2-fluoro-4-chloro-5-isopropoxyphenyl]-4-methyl-5-trifluoromethylpyridazin-3-one was dissolved in about 10 ml of concentrated sulfuric acid under ice cooling, and the solution was warmed to room temperature. After ten minutes, about 100 ml of water was added to the reaction mixture. The deposited crystals were collected by filtration, and then washed twice with 20 ml of water and once with 10 ml of hexane in this order. The crystals thus obtained were recrystallized from isopropanol, which afforded 3.2 g (9.9 mmol) of 2-[2-fluoro-4-chloro-5-hydroxy-phenyl]-4-methyl-5-trifluoromethylpyridazin-3-one.

후처리

  1. waitAfter ten minutes
  2. filtrationThe deposited crystals were collected by filtration
  3. washwashed twice with 20 ml of water and once with 10 ml of hexane in this order
  4. customThe crystals thus obtained
  5. customwere recrystallized from isopropanol, which

출처 및 근거

ORD 기록
ord-52a57115931245ce99bfe8e7f9b71474
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06022829

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