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盐酸 → HCID 178433880,化合物

HRID 910331
笔记
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反应方程式

HRID 910331 反应方程式
[NH2:1][C:2]1[C:3]([OH:17])=[C:4]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([OH:16])=[O:15])[CH:9]=2)[CH:5]=[CH:6][CH:7]=1.Cl.N([O-])=O.[Na+].S(=O)(=O)(O)[NH2:24].[CH3:28][C:29]1[CH:30]=[C:31]([N:36]2[C:40]([OH:41])=[CH:39][C:38]([CH3:42])=[N:37]2)[CH:32]=[CH:33][C:34]=1[CH3:35]>O.C(N(CC)CC)C.CO>[CH3:35][C:34]1[CH:33]=[CH:32][C:31]([N:36]2[N:37]=[C:38]([CH3:42])/[C:39](=[N:24]/[NH:1][C:2]3[CH:7]=[CH:6][CH:5]=[C:4]([C:8]4[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([OH:16])=[O:15])[CH:9]=4)[C:3]=3[OH:17])/[C:40]2=[O:41])=[CH:30][C:29]=1[CH3:28]
参与物实验过程后处理来源与证据反应笔记

参与物

9

反应物 5

HCID 313盐酸2 次HCID 5987氨基磺酸HCID 114923323'-氨基-2'-羟基-[1,1'-联苯]-3-甲酸HCID 23668193亚硝酸钠HCID 178429255HCID 178429255,化合物

产物 1

HCID 178433880HCID 178433880,化合物收率 95.4%

试剂、催化剂与溶剂 3

HCID 887
Methanol
溶剂
HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂2 次
HCID 8471三乙胺溶剂

实验过程

3′-Amino-2′-hydroxybiphenyl-3-carboxylic acid (“BPCA”) Form I (90 g, 392.6 mmol), was added slowly with stirring at room temperature to a solvent mixture of tech. methanol (1.8 L) and 4 M hydrochloric acid (0.245 L, 981.5 mmol) in 3 L reactor. The resulting red solution was stirred for thirty minutes. The solution was then cooled to 0-5° C. and a cold solution of sodium nitrite (27 g, 391.3 mmol) in 90 mL of water was added over twenty minutes such that the reaction mixture temperature did not rise above 10° C. The reaction mixture was stirred for one hour at 5-10° C. Sulfamic acid (4 g, 41.2 mmol) in 90 mL of water was added at 5° C. and the resulting mixture was stirred for additionally one hour at the same temperature. The reaction mixture was warmed to room temperature and triethylamine (ca 104 mL) was added to adjust pH 7-8. 1-(3,4-dimethylphenyl)-3-methyl-1H-pyrazol-5-ol (“pyrazole”) form I (72 g, 357.8 mmol), was added in one portion to the reaction mixture and the resulting mixture was stirred for additionally two hours at room temperature. Hydrochloric acid (4M, ca 140 mL) was slowly added with stirring over twenty minutes to adjust pH to 1.8. A solid precipitated and was collected by filtration, washed with of mixture MeOH:water (1:1, 100 mL) and dried at 40° C./0 bar in vacuum oven for about 18 hours giving 151 g of crude orange to brown crystals of Eltrombopag crude (XRPD: form III with small percentage (less than 10%) of form I. (HPLC: 98.5%, Yield=95.4%)

后处理

  1. stirringThe resulting red solution was stirred for thirty minutes
  2. temperatureThe solution was then cooled to 0-5° C.
  3. customdid not rise above 10° C
  4. stirringThe reaction mixture was stirred for one hour at 5-10° C
  5. stirringthe resulting mixture was stirred for additionally one hour at the same temperature
  6. temperatureThe reaction mixture was warmed to room temperature
  7. stirringthe resulting mixture was stirred for additionally two hours at room temperature
  8. stirringwith stirring over twenty minutes
  9. customA solid precipitated
  10. filtrationwas collected by filtration
  11. washwashed with of mixture MeOH:water (1:1, 100 mL)
  12. customdried at 40° C./0 bar in vacuum oven for about 18 hours

来源与证据

ORD记录
ord-e836008021224355bf21c4f1801f77ca
来源数据集
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08022093B2

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记