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Sodium Bicarbonate → HCID 178433801, 화합물

HRID 384391
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HRID 384391 반응식
Br.[OH:2][C:3]1[C:8]([NH2:9])=[CH:7][CH:6]=[CH:5][C:4]=1[C:10]1[S:11][C:12]([CH3:18])=[C:13]([C:15]([OH:17])=[O:16])[N:14]=1.[N:19]([O-])=O.[Na+].[CH2:23]1[C:31]2[C:26](=[CH:27][C:28]([N:32]3[C:36](=[O:37])[CH2:35][C:34]([CH3:38])=[N:33]3)=[CH:29][CH:30]=2)[CH2:25][CH2:24]1.C(=O)(O)[O-].[Na+]>Cl>[OH:2][C:3]1[C:8]([NH:9][N:19]=[C:35]2[C:36](=[O:37])[N:32]([C:28]3[CH:27]=[C:26]4[C:31](=[CH:30][CH:29]=3)[CH2:23][CH2:24][CH2:25]4)[N:33]=[C:34]2[CH3:38])=[CH:7][CH:6]=[CH:5][C:4]=1[C:10]1[S:11][C:12]([CH3:18])=[C:13]([C:15]([OH:17])=[O:16])[N:14]=1
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참가 물질

6

반응물 4

HCID 516892Sodium BicarbonateHCID 23668193Sodium NitriteHCID 574837802-Indan-5-yl-5-methyl-2,4-dihydro-pyrazol-3-oneHCID 136117081HCID 136117081, 화합물

생성물 1

HCID 178433801HCID 178433801, 화합물수율 75.9%

시약·촉매·용매 1

HCID 313
Hydrochloric Acid
용매

실험 절차

2-(2-Hydroxy-3-amino-phenyl)-5-methyl-thiazole-4-carboxylic acid hydrobromide 47c (200 mg, 0.60 mmol) was dissolved in 2 mL of hydrochloric acid (1 N) upon cooling by an ice-water bath, followed by dropwise addition of 0.82 mL of aqueous sodium nitrite (46 mg, 0.66 mmol). After the mixture was stirred for 20 minutes, 2-indan-5-yl-5-methyl-2,4-dihydro-pyrazol-3-one 1i (116 mg, 0.544 mmol) was added. The mixture was adjusted to pH 8˜9 by batch addition of saturated aqueous sodium bicarbonate (781 mg, 9.3 mmol). Then the generated bubbles were quenched with 2 mL of ethanol. The reaction mixture was warmed up to room temperature and reacted overnight. The reaction was monitored by TLC until the disappearance of the starting materials. The mixture was filtered and the filter cake was dissolved in 20 mL of water. The mixture was adjusted to pH 3˜4 with concentrated hydrochloric acid. The mixture was filtered and the filter cake was dried and purified by HPLC to obtain the title compound 2-{2-hydroxy-3-[N′-(1-indan-5-yl-3-methyl-5-oxo-1,5-dihydro-pyrazol-4-ylidene)-hydrazino]-phenyl}-5-methyl-thiazole-4-carboxylic acid 47 (195 mg, yield 75.9%) as a red solid.

후처리

  1. temperatureupon cooling by an ice-water bath
  2. customThen the generated bubbles were quenched with 2 mL of ethanol
  3. customreacted overnight
  4. filtrationThe mixture was filtered
  5. dissolutionthe filter cake was dissolved in 20 mL of water
  6. filtrationThe mixture was filtered
  7. customthe filter cake was dried
  8. custompurified by HPLC

출처 및 근거

ORD 기록
ord-14321b6d8c214ebf8b142965e1fcaa63
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08367710B2

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