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Acetic Acid → HCID 178514959, 화합물

HRID 1951290
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HRID 1951290 반응식
[NH2:1][C:2]1[CH:6]=[C:5]([OH:7])[NH:4][N:3]=1.[C:8]1(=O)[O:13][C:11](=[O:12])[C:10]2=[CH:14][CH:15]=[CH:16][CH:17]=[C:9]12.C(O)(=O)C>C1COCC1>[OH:7][C:5]1[NH:4][N:3]=[C:2]([N:1]2[C:11](=[O:12])[C:10]3[C:9](=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:8]2=[O:13])[CH:6]=1
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참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 6811Phthalic AnhydrideHCID 962213-Amino-5-hydroxypyrazole

생성물 1

HCID 178514959HCID 178514959, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

To a solution of 3-amino-1H-pyrazol-5-ol (10.00 g, 101 mmol) in THF (300 mL) at RT was added phthalic acid anhydride (14.9 g, 101 mmol) followed by acetic acid (69.3 ml, 1.21 mol). The mixture was heated to reflux. After 4 days, the mixture was concentrated in vacuo to afford a slurry that was cooled to 0° C. and filtered. The solid was rinsed with Et2O and dried in vacuo to afford 2-(5-hydroxy-1H-pyrazol-3-yl)isoindoline-1,3-dione as a yellow solid that was advanced without further purification. MS: Found M+H+=230.2.

후처리

  1. temperatureThe mixture was heated to reflux
  2. concentrationthe mixture was concentrated in vacuo
  3. customto afford a slurry that
  4. filtrationfiltered
  5. washThe solid was rinsed with Et2O
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-2c128b4fcd084ed586a683b37ed74654
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08404694B2

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