Hydrochloric Acid → HCID 12850756、化合物

HRID 1395041ノート

反応式

HRID 1395041 の反応式
C([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:11]=[CH:12][C:13]3[C:19](=[O:20])[C:18]([C:21]([O:23]CC)=[O:22])=[CH:17][NH:16][C:14]=3[N:15]=2)[CH2:6][CH2:5]1)(=O)C.Cl>O.C(O)C>[N:7]1([C:10]2[N:11]=[CH:12][C:13]3[C:19](=[O:20])[C:18]([C:21]([OH:23])=[O:22])=[CH:17][NH:16][C:14]=3[N:15]=2)[CH2:6][CH2:5][NH:4][CH2:9][CH2:8]1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 12917681Ethyl 2-(4-acetyl-1-piperazinyl)-5,8-dihydro-5-oxopyrido[2,3-d]pyrimidine-6-carboxylate

生成物 1

HCID 12850756HCID 12850756、化合物収率 78.4%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A suspension of ethyl 5,8-dihydro-2-(4-acetyl-1-piperazinyl)-5-oxopyrido[2,3-d]pyrimidine-6-carboxylate (1000 g) and concentrated hydrochloric acid (800 ml) in a mixture of water (1200 ml) and ethanol (1000 ml) was refluxed for 8 hours and allowed to stand overnight. The crystals precipitated were collected, washed with ethanol, and dissolved by heating in an aqueous solution (10 liters) of sodium hydroxide (250 g). The solution was filtered, adjusted to pH 7-8 with acetic acid, and allowed to stand overnight with ice-cooling. The crystalline precipitate was collected, washed with water, and dried at 110° C. to give 5,8-dihydro-2-(1-piperazinyl)-5-oxopyrido [2,3-d]pyrimidine-6-carboxylic acid (625 g). m.p. 299°-305° C. (decomp.).

後処理

  1. temperaturewas refluxed for 8 hours
  2. customThe crystals precipitated
  3. customwere collected
  4. washwashed with ethanol
  5. dissolutiondissolved
  6. temperatureby heating in an aqueous solution (10 liters) of sodium hydroxide (250 g)
  7. filtrationThe solution was filtered
  8. waitto stand overnight with ice-
  9. temperaturecooling
  10. customThe crystalline precipitate was collected
  11. washwashed with water
  12. customdried at 110° C.

出典と根拠

ORDレコード
ord-42f90dcbb8e648d994227d86eda3b2f5
出典データセット
uspto-grants-1980_05
特許番号
US04201781

反応ノート

読み込み中…