Isoamyl Alcohol → HCID 70625226, 화합물

HRID 65991노트

반응식

HRID 65991 반응식
[Na].[CH3:2][CH:3]([CH3:7])[CH2:4][CH2:5][OH:6].Cl[C:9]1[C:10]2[C:11](=[N:21][N:22]([CH3:24])[CH:23]=2)[N:12]=[C:13]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:14]=1.[C:25]([OH:32])(=[O:31])/[CH:26]=[CH:27]\[C:28]([OH:30])=[O:29]>CCOCC.O>[C:25]([OH:32])(=[O:31])/[CH:26]=[CH:27]\[C:28]([OH:30])=[O:29].[CH3:24][N:22]1[CH:23]=[C:10]2[C:11]([N:12]=[C:13]([C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:14]=[C:9]2[O:6][CH2:5][CH2:4][CH:3]([CH3:7])[CH3:2])=[N:21]1

참가 물질

7

반응물 4

HCID 31260Isoamyl AlcoholHCID 444266Maleic AcidHCID 5360545SodiumHCID 22756855HCID 22756855, 화합물

생성물 1

HCID 70625226HCID 70625226, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 3283Diethyl Ether용매2회

실험 절차

To a solution of 1.61 g. of sodium (0.07 mol.) in 200 ml. of 3-methyl butanol, 17.1 g. of 4-chloro-2-methyl-6-phenyl-2H-pyrazolo[3,4-b]pyridine (0.07 mol.) are added and the mixture is refluxed for six hours while stirring. The cooled solution is agitated with water, the organic layer dried and then evaporated in vacuo to give 20 g. (97%) of oil. To 18.5 g. of the oil (0.063 mol.), dissolved in 50 ml. of ether, a solution of 14.6 g. of maleic acid (0.126 mol.) in 500 ml. of ether is added. The precipitated maleate of 2-methyl-4-(3-methylbutoxy)-6-phenyl-2H-pyrazolo [3,4-b]pyridine, at first oily, crystallizes on standing overnight, yield: 24.6 g. (83%); m.p. 114°-116°. Recrystallization from ethyl acetate gives a product which melts at 119°-120°.

후처리

  1. temperaturethe mixture is refluxed for six hours
  2. customthe organic layer dried
  3. customevaporated in vacuo
  4. customto give 20 g
  5. dissolutionof the oil (0.063 mol.), dissolved in 50 ml
  6. customThe precipitated maleate of 2-methyl-4-(3-methylbutoxy)-6-phenyl-2H-pyrazolo [3,4-b]pyridine, at first oily, crystallizes
  7. customRecrystallization from ethyl acetate
  8. customgives a product which melts at 119°-120°

출처 및 근거

ORD 기록
ord-69b56ea87f7d4a50a49798b3cbfd0d3d
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04129738

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