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Triethylamine → HCID 44607520、化合物

HRID 1372790
ノート
印刷プレビュー

反応式

HRID 1372790 の反応式
[CH3:1][O:2][C:3]1[CH:21]=[CH:20][C:6]([CH2:7][N:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]([C:17]([OH:19])=O)=[N:9]2)=[CH:5][CH:4]=1.C(Cl)(=O)C(Cl)=O.[NH2:28][C:29]1[C:34]([Cl:35])=[CH:33][C:32]([CH2:36][C:37]([O:39][CH2:40][CH3:41])=[O:38])=[C:31]([F:42])[CH:30]=1.C(N(CC)CC)C>C(Cl)Cl.CN(C=O)C.O>[Cl:35][C:34]1[C:29]([NH:28][C:17]([C:10]2[C:11]3[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=3)[N:8]([CH2:7][C:6]3[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:21][CH:20]=3)[N:9]=2)=[O:19])=[CH:30][C:31]([F:42])=[C:32]([CH2:36][C:37]([O:39][CH2:40][CH3:41])=[O:38])[CH:33]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 17858807Ethyl 4-amino-5-chloro-2-fluorophenylacetateHCID 178594441-((4-methoxyphenyl)methyl)-1H-indazole-3-carboxylic acid

生成物 1

HCID 44607520HCID 44607520、化合物収率 80%

試薬・触媒・溶媒 3

HCID 6228
Dimethylformamide
触媒
HCID 962Water溶媒
HCID 6344Dichloromethane溶媒

実験手順

In methylene chloride (10 ml) was dissolved 1-(4-methoxybenzyl)-3-indazolylcarboxylic acid (630 mg, 2.23 mmol). To the resulting solution were added oxalyl chloride (292 μl, 3.53 mmol) and DMF (1 drop). The resulting mixture was stirred until the mixture became uniform. From the reaction mixture, the solvent was distilled off under reduced pressure. The residue was dissolved in methylene chloride (20 ml). Ethyl (4-amino-5-chloro-2-fluorophenyl)acetate (517 mg, 2.23 mmol) and triethylamine (621 μl, 4.46 mmol) were added to the resulting solution. The resulting mixture was heated under reflux for 15 hours. After cooling, the reaction mixture was added with water (50 ml), followed by extraction with chloroform (200 ml). The extract was dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent. The residue was purified by chromatography on a silica gel column, whereby from hexane-ethyl acetate (4:1) eluate fractions, ethyl (5-chloro-2-fluoro-4-(1-(4-methoxybenzyl)-3-indazolylcarbonylamino)phenyl)acetate (881 mg, 80%) was obtained as a pale yellow amorphous substance.

後処理

  1. distillationFrom the reaction mixture, the solvent was distilled off under reduced pressure
  2. dissolutionThe residue was dissolved in methylene chloride (20 ml)
  3. temperatureThe resulting mixture was heated
  4. temperatureunder reflux for 15 hours
  5. temperatureAfter cooling
  6. extractionfollowed by extraction with chloroform (200 ml)
  7. dry with materialThe extract was dried over anhydrous magnesium sulfate
  8. distillationdistilled under reduced pressure
  9. customto remove the solvent
  10. customThe residue was purified by chromatography on a silica gel column, whereby from hexane-ethyl acetate (4:1) eluate fractions

出典と根拠

ORDレコード
ord-64b3635a170d46b38d678f7ccc43fbfc
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07157487B2

反応ノート

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