Ethanol → 5,8-Dihydro-2-(1-piperazinyl)-8-vinyl-5-oxopyrido[2,3-d]pyrimidine-6-carboxylic acid hydrochloride

HRID 1658139ノート

反応式

HRID 1658139 の反応式
C(O)C.[H-].[Na+].C([N:9]1[CH2:14][CH2:13][N:12]([C:15]2[N:16]=[CH:17][C:18]3[C:24](=[O:25])[C:23]([C:26]([O:28]CC)=[O:27])=[CH:22][N:21]([CH2:31][CH2:32][Cl:33])[C:19]=3[N:20]=2)[CH2:11][CH2:10]1)(=O)C>O>[ClH:33].[N:12]1([C:15]2[N:16]=[CH:17][C:18]3[C:24](=[O:25])[C:23]([C:26]([OH:28])=[O:27])=[CH:22][N:21]([CH:31]=[CH2:32])[C:19]=3[N:20]=2)[CH2:11][CH2:10][NH:9][CH2:14][CH2:13]1

参加物

5

反応物 3

HCID 702EthanolHCID 24758Sodium hydrideHCID 13334740Ethyl 2-(4-acetyl-1-piperazinyl)-8-(2-chloroethyl)-5,8-dihydro-5-oxopyrido[2,3-d]-pyrimidine-6-carboxylate

生成物 1

HCID 123790215,8-Dihydro-2-(1-piperazinyl)-8-vinyl-5-oxopyrido[2,3-d]pyrimidine-6-carboxylic acid hydrochloride収率 67.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a mixture, containing 400 ml of absolute ethanol and 2.0 g of 65% sodium hydride, which was held at 60°C was added with stirring 5.0 g of ethyl 2-(4-acetyl-1-piperazinyl)-8-(2-chloroethyl)-5,8-dihydro-5oxopyrido[2,3-d]pyrimidine-6-carboxylate. The resulting mixture was heated to reflux for 2 hours and at the end of the period 200 ml of water was added. The mixture was refluxed for an additional 30 minutes. The ethanol was distilled off under reduced pressure and the resulting residue was acidified with concentrated hydrochloric acid to pH 1.0. The resulting precipitate was collected and recrystallized from water to yield 2.8 g of the product, m.p 298° - 301°C with decomposition.

後処理

  1. customwas held at 60°C
  2. additionwas added
  3. temperatureThe resulting mixture was heated
  4. additionwas added
  5. temperatureThe mixture was refluxed for an additional 30 minutes
  6. distillationThe ethanol was distilled off under reduced pressure
  7. customThe resulting precipitate was collected
  8. customrecrystallized from water

出典と根拠

ORDレコード
ord-1b693982a9d841e2850a56eb795798c4
出典データセット
uspto-grants-1976_06
特許番号
US03962443

反応ノート

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