1-(1H-pyrrolo[2,3-c]pyridin-2-yl)ethanone → HCID 178465622、化合物

HRID 1821868ノート

反応式

HRID 1821868 の反応式
[NH:1]1[C:5]2=[CH:6][N:7]=[CH:8][CH:9]=[C:4]2[CH:3]=[C:2]1[C:10](=O)[CH3:11].[C:13]([NH:16][NH2:17])([NH2:15])=[NH:14].[ClH:18]>C(O)C.Cl>[ClH:18].[ClH:18].[NH:1]1[C:5]2=[CH:6][N:7]=[CH:8][CH:9]=[C:4]2[CH:3]=[C:2]1[C:10](=[N:17][NH:16][C:13]([NH2:15])=[NH:14])[CH3:11]

参加物

5

反応物 2

HCID 552679001-(1H-pyrrolo[2,3-c]pyridin-2-yl)ethanoneHCID 178418668HCID 178418668、化合物

生成物 1

HCID 178465622HCID 178465622、化合物収率 161.8%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 702Ethanol溶媒

実験手順

A mixture of 1-(1H-pyrrolo[2,3-c]pyridin-2-yl)ethanone (Example 70) (90 mg, 0.56 mmol) and aminoguanidine hydrochloride (65 mg, 0.59 mmol) in ethanol (5.6 mL) and 6 N HCl (0.47 mL) was heated under reflux for 1.5 h. The reaction mixture was cooled to room temperature and the precipitate was filtered, rinsed with ethanol and diethyl ether, and dried under vacuum at 45° C. to provide [[1-(1H-pyrrolo[2,3-c]pyridin-2-yl)ethylidene]amino]guanidine dihydrochloride (138 mg, 86%) as a white solid: mp 314-318° C. dec.; 1H NMR (300 MHz, CD3OD) δ2.50 (3H, s), 7.40 (1H, s), 8.10-8.27 (2H, m), 9.04 (1H, s); ESI MS m/z 217 [C10H12N6+H]+; HPLC (Method A) >99% (AUC), tR=9.01 min.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 1.5 h
  3. filtrationthe precipitate was filtered
  4. washrinsed with ethanol and diethyl ether
  5. customdried under vacuum at 45° C.

出典と根拠

ORDレコード
ord-ea8ba445279a461ca1eab23e704a9187
出典データセット
uspto-grants-2009_10
特許番号
US07608627B2

反応ノート

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