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Acetic Anhydride → 1-(2-acetoxyethyl)-3-(3,5-di-tertiary butylphenyl)-1H-pyrazolo[3,4-b]pyridine

HRID 1382893
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HRID 1382893 반응식
[C:1]([C:5]1[CH:6]=[C:7]([C:16]2[C:24]3[C:19](=[N:20][CH:21]=[CH:22][CH:23]=3)[N:18]([CH2:25][CH2:26][OH:27])[N:17]=2)[CH:8]=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:10]=1O)([CH3:4])([CH3:3])[CH3:2].[C:28](OC(=O)C)(=[O:30])[CH3:29]>C1(C)C=CC=CC=1>[C:28]([O:27][CH2:26][CH2:25][N:18]1[C:19]2=[N:20][CH:21]=[CH:22][CH:23]=[C:24]2[C:16]([C:7]2[CH:6]=[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[CH:10]=[C:9]([C:12]([CH3:14])([CH3:13])[CH3:15])[CH:8]=2)=[N:17]1)(=[O:30])[CH3:29]
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참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 30873781H-Pyrazolo(3,4-b)pyridine-1-ethanol, 3-(3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl)-

생성물 1

HCID 212736381-(2-acetoxyethyl)-3-(3,5-di-tertiary butylphenyl)-1H-pyrazolo[3,4-b]pyridine수율 86.4%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
20 °C

실험 절차

To a solution of 40 g of the compound of Example 43 in 320 ml of toluene is added 22 g of acetic anhydride under stirring, and refluxed for 8 hours. After completion of the reaction, the reaction mixture is cooled to 20° C., washed with 300 ml of water twice and dried over anhydrous sodium sulfate. The toluene is concentrated and the residue is recrystallized from ethanol and dried to give 37 g of 1-(2-acetoxyethyl)-3-(3,5-di-tertiary butylphenyl)-1H-pyrazolo[3,4-b]pyridine, melting at 115°-116° C.

후처리

  1. temperaturerefluxed for 8 hours
  2. customAfter completion of the reaction
  3. washwashed with 300 ml of water twice
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationThe toluene is concentrated
  6. customthe residue is recrystallized from ethanol
  7. customdried

출처 및 근거

ORD 기록
ord-3db335a915d04e1c83ac3dd8cedd4b8c
출처 데이터셋
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04808620

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