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Hydrochloric Acid → 3-amino-5-(5-methyl-1H-pyrazol-4-yl)thiophene-2-carboxamide

HRID 2364073
ノート
印刷プレビュー

反応式

HRID 2364073 の反応式
CC1(C)[NH:7][C:6]2[CH:8]=[C:9]([C:11]3[CH:12]=[N:13][NH:14][C:15]=3[CH3:16])[S:10][C:5]=2[C:4](=[O:17])[NH:3]1.Cl>CO>[NH2:7][C:6]1[CH:8]=[C:9]([C:11]2[CH:12]=[N:13][NH:14][C:15]=2[CH3:16])[S:10][C:5]=1[C:4]([NH2:3])=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 66743505Cdc7-IN-15

生成物 1

HCID 667430133-amino-5-(5-methyl-1H-pyrazol-4-yl)thiophene-2-carboxamide収率 72%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 2,2-dimethyl-6-(5-methyl-1H-pyrazol-4-yl)-2,3-dihydrothieno[3,2-d]pyrimidin-4(1H)-one (1.97 g, 7.51 mmol), 1 M aqueous HCl. (38 mL) and MeOH (38 mL) was stirred at 50° C. for 4 h. After removal of the solvent at reduced pressure, the organic materials were extracted with EtOAc/THF. The combined extracts were dried over Na2SO4 and filtered. After removal of the solvent at reduced pressure, the residue was purified by column chromatography (Purif, silica gel, EtOAc to 90:10 EtOAc/MeOH) to give the title compound (1.20 g, 72%) as a green solid:

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. customAfter removal of the solvent at reduced pressure
  2. extractionthe organic materials were extracted with EtOAc/THF
  3. dry with materialThe combined extracts were dried over Na2SO4
  4. filtrationfiltered
  5. customAfter removal of the solvent at reduced pressure
  6. customthe residue was purified by column chromatography (Purif, silica gel, EtOAc to 90:10 EtOAc/MeOH)

出典と根拠

ORDレコード
ord-d365f5cec34a4d97ab8567ace77df18c
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08691828B2

反応ノート

読み込み中…