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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 178433880, 화합물 → HCID 178433881, 화합물

HRID 386366
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HRID 386366 반응식
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([N:9]2[N:32]=[C:31]([CH3:33])/[C:12](=[N:13]/[NH:14][C:15]3[CH:16]=[CH:17][CH:18]=[C:19]([C:22]4[CH:23]=[CH:24][CH:25]=[C:26]([C:28]([OH:30])=[O:29])[CH:27]=4)[C:20]=3[OH:21])/[C:10]2=[O:11])=[CH:6][C:7]=1[CH3:8]>C(O)(=O)C>[CH3:8][C:7]1[CH:6]=[C:5]([N:9]2[C:10](=[O:11])[C:12](=[N:13][NH:14][C:15]3[C:20]([OH:21])=[C:19]([C:22]4[CH:23]=[CH:24][CH:25]=[C:26]([C:28]([OH:30])=[O:29])[CH:27]=4)[CH:18]=[CH:17][CH:16]=3)[C:31]([CH3:33])=[N:32]2)[CH:4]=[CH:3][C:2]=1[CH3:1]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 178433880HCID 178433880, 화합물

생성물 1

HCID 178433881HCID 178433881, 화합물수율 88%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
40 °C

실험 절차

Crude Eltrombopag (151 g, HPLC purity: 98.5%) was suspended in 2.9 L of glacial acetic acid in 3 L reactor. The suspension was stirred for five hours under reflux and cooled to 40° C. Crystals formed and were filtrated off, washed with 200 mL of methanol:water (1:1) and dried at 60° C./0 mbar overnight yielding 133 g orange solid of pure 3′-{N′-[1-(3,4-Dimethylphenyl)-3-methyl-5-oxo-1,5-dihydro-pyrazol-4-ylidene]hydrazino}-2′-hydroxybiphenyl-3-carboxylic acid (HPLC: 99.8%; XRPD: form I) (Yield=88%). PXRD analysis provided the diffractogram as shown in FIG. 1. DSC analysis provided the thermogram as shown in FIG. 2

후처리

  1. temperatureunder reflux
  2. customCrystals formed
  3. filtrationwere filtrated off
  4. washwashed with 200 mL of methanol:water (1:1)
  5. customdried at 60° C./0 mbar overnight

출처 및 근거

ORD 기록
ord-db4836d8a1be4b68aadde99eb2e28755
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08372822B2

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