Hydrogen Peroxide → 1-(3,5-Dichloro-pyridin-4-ylmethyl)-6-methoxy-4-[1,2,4]triazol-1-yl-phthalazine 3-oxide

HRID 2268894노트

반응식

HRID 2268894 반응식
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:26])[C:7]=1[CH2:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([O:19][CH3:20])=[CH:16][CH:17]=2)[C:12]([N:21]2[CH:25]=[N:24][CH:23]=[N:22]2)=[N:11][N:10]=1.OO.[OH-].[Na+].C(OCC)(=[O:33])C.C(OCC)C>FC(F)(F)C(O)=O>[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:26])[C:7]=1[CH2:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([O:19][CH3:20])=[CH:16][CH:17]=2)[C:12]([N:21]2[CH:25]=[N:24][CH:23]=[N:22]2)=[N+:11]([O-:33])[N:10]=1

참가 물질

6

반응물 4

HCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 98215811-(3,5-Dichloro-pyridin-4-ylmethyl)-6-methoxy-4-[1,2,4]triazol-1-yl-phthalazineHCID 21584169Diethylether ethylacetate

생성물 1

HCID 183816001-(3,5-Dichloro-pyridin-4-ylmethyl)-6-methoxy-4-[1,2,4]triazol-1-yl-phthalazine 3-oxide수율 41%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

Under N2 at 0° C. a solution of 1-(3,5-dichloro-pyridin-4-ylmethyl)-6-methoxy-4-[1,2,4]triazol-1-yl-phthalazine (5.1 g, 13.2 mmoles), prepared as described in example 51, in trifluoroacetic acid (25 ml), was dropwise added with H2O2 (1.35 ml, 13.5 mmoles). The temperature was left to rise to the room value and, after 48 hours, the pH was adjusted with NaOH. After further 24 hours under stirring, the mixture was dried, taken up in CH2Cl2. The organic phase was washed with water, anhydrified and dried to give a foam which was flash chromatographed (eluent: ethyl acetate/ethyl ether 6:4, then 8:2) to give 2.2 g of the title compound (yield: 41%). m.p.: 218-220° C. (dec.).

후처리

  1. waitThe temperature was left
  2. customthe mixture was dried
  3. washThe organic phase was washed with water
  4. customdried
  5. customto give a foam which
  6. customchromatographed (eluent

출처 및 근거

ORD 기록
ord-a4d6762e8e034609b279434239d47de0
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06329370B1

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