Hydrochloric Acid → HCID 12818612、化合物

HRID 2285815ノート

反応式

HRID 2285815 の反応式
[CH2:1]([O:3][C:4]([C:6]1[C:7](=[O:19])[N:8]([CH3:18])[C:9]2[C:14]([C:15]=1Cl)=[CH:13][CH:12]=[C:11]([CH3:17])[N:10]=2)=[O:5])[CH3:2].[CH3:20][N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1.C(=O)([O-])[O-].[Na+].[Na+].Cl>C(O)C>[CH2:1]([O:3][C:4]([C:6]1[C:7](=[O:19])[N:8]([CH3:18])[C:9]2[C:14]([C:15]=1[N:24]1[CH2:25][CH2:26][N:21]([CH3:20])[CH2:22][CH2:23]1)=[CH:13][CH:12]=[C:11]([CH3:17])[N:10]=2)=[O:5])[CH3:2]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 531671-MethylpiperazineHCID 12818608HCID 12818608、化合物

生成物 1

HCID 12818612HCID 12818612、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A stirred mixture of 5.3 g. (0.019 mole) of 4-chloro-1,7-dimethyl-1,2-dihydro-2-oxo-1,8-naphthyridine-3-carboxylic acid ethyl ester, 1.9 g. (0.019 mole) of N-methylpiperazine and 1.9 g. (0.019 mole) of sodium carbonate in 100 ml. of ethanol was heated under reflux for 5 hours. The mixture was filtered and the filtrate was evaporated in a rotary evaporator. The residue was triturated with 150 ml. of 10% aqueous sodium carbonate and was extracted with 150 ml. of ether. The ether layer was dried over magnesium sulfate, filtered and was diluted with 30 ml. of ethanol. This solution was acidified with an ethereal hydrochloric acid solution. The precipitate which formed was collected and was recrystallized from ethanol to afford 1.0 g. of product as the hydrochloride, hemihydrate, m.p. 278°-280° C. dec.

後処理

  1. additionA stirred mixture of 5.3 g
  2. temperatureunder reflux for 5 hours
  3. filtrationThe mixture was filtered
  4. customthe filtrate was evaporated in a rotary evaporator
  5. customThe residue was triturated with 150 ml
  6. extractionof 10% aqueous sodium carbonate and was extracted with 150 ml
  7. dry with materialThe ether layer was dried over magnesium sulfate
  8. filtrationfiltered
  9. additionwas diluted with 30 ml
  10. customThe precipitate which formed
  11. customwas collected
  12. customwas recrystallized from ethanol
  13. customto afford 1.0 g

出典と根拠

ORDレコード
ord-cacf838e5b794b6aa0b369ddf0432c90
出典データセット
uspto-grants-1982_04
特許番号
US04324893

反応ノート

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