Hydrazine hydrate (1:1) → HCID 135519368, 화합물

HRID 1296956노트

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HRID 1296956 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[OH:12])[O:8][C:7]([C:13]([OH:15])=[O:14])=[C:6]([C:16]1[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=1)[C:5]2=O.O.[NH2:26][NH2:27]>C(O)C.C([O-])(O)=O.[Na+]>[Cl:1][C:2]1[C:11]([OH:12])=[CH:10][C:9]([OH:8])=[C:4]([C:5]2[C:6]([C:16]3[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=3)=[C:7]([C:13]([OH:15])=[O:14])[NH:26][N:27]=2)[CH:3]=1

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 11416722HCID 11416722, 화합물

생성물 1

HCID 135519368HCID 135519368, 화합물

시약·촉매·용매 2

HCID 516892Sodium Bicarbonate촉매HCID 702Ethanol용매

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온도
70 °C

실험 절차

6-Chloro-7-hydroxy-3-(4-methoxy-phenyl)-4-oxo-4H-chromene-2-carboxylic acid (1 eq) was taken up in ethanol and hydrazine hydrate (3 eq) was added. To aid dissolution a few drops of NaHCO3 (aq) was added, and then all was heated at 70° C. under nitrogen for 2 hours. The solution was cooled to room temperature and concentrated in vacuo to a brown oil. This was partitioned between 1M HCl (aq) and diethyl ether. The organic phases were combined, washed with 1M HCl (aq), dried over MgSO4, filtered and concentrated in vacuo to give 5-(5-chloro-2,4-dihydroxy-phenyl)-4-(4-methoxy-phenyl)-2H-pyrazole-3-carboxylic acid as a yellow foam.

후처리

  1. additionwas added
  2. temperatureThe solution was cooled to room temperature
  3. concentrationconcentrated in vacuo to a brown oil
  4. customThis was partitioned between 1M HCl (aq) and diethyl ether
  5. washwashed with 1M HCl (aq)
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-98a05657a50a4ebb8193f511c258c0f6
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07247734B2

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