Ammonium Hydroxide → HCID 178516745、化合物

HRID 1762098ノート

反応式

HRID 1762098 の反応式
[NH2:1][C:2]1[NH:6][N:5]=[C:4]([N:7]2[CH2:12][CH2:11][O:10][CH2:9][CH2:8]2)[N:3]=1.Cl.[CH2:14]([N:21]1[CH2:26][CH2:25][C:24](=O)[CH:23]([C:28](OC)=O)[CH2:22]1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[OH-:32].[NH4+]>C(O)(=O)C>[CH2:14]([N:21]1[CH2:26][C:25](=[O:32])[C:24]2[N:1]=[C:2]3[N:3]=[C:4]([N:7]4[CH2:8][CH2:9][O:10][CH2:11][CH2:12]4)[NH:5][N:6]3[CH2:28][C:23]=2[CH2:22]1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 14923Ammonium HydroxideHCID 107479Methyl 1-benzyl-4-oxopiperidine-3-carboxylate hydrochlorideHCID 44173793-morpholin-4-yl-1H-1,2,4-triazol-5-amine

生成物 1

HCID 178516745HCID 178516745、化合物収率 72%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 50.76 g (0.3 mole) of 5-amino-3-morpholino-1H-1,2,4-triazole, 85.13 g (0.3 mole) of 1-benzyl-3-carbomethoxy-4-piperidone-hydrochloride and 175 ml of acetic acid is heated to boiling for 6 hours. After cooling 400 ml of concentrated ammonium hydroxide solution are added to the reaction mixture, which is then allowed to stand at room temperature for 16 hours. The precipitated crystals are filtered and washed with 200 ml of water. The product is heated to boiling in 500 ml of methanol for 15 minutes, filtered, washed with 400 ml of methanol, dissolved in hot dimethyl formamide, precipitated by adding acetonitrile, filtered and washed with acetonitrile. Thus 78.81 g of 7-benzyl-2-morpholino-6,7,8,9-tetrahydro-pyrido[4,3-d]-1,2,4-triazolo[1,5-a]pyrimidine-5(10H)-one are obtained, yield 72%, m.p.: 291°-293° C. The crystals precipitated from the methanol solution are filtered, washed with methanol, dissolved in 60 ml of hot dimethyl formamide, precipitated by adding 60 ml of acetonitrile, filtered and washed with acetonitrile. Thus 6.63 g of 7-benzyl-2-morpholino-6,7,8,9-tetrahydro-pyrido[4,3-d]-1,2,4-triazolo[1,5-a]pyrimidine-6(10H)-one are obtained, yield 6%, m.p.: 252°-254° C.

後処理

  1. temperatureis heated
  2. additionare added to the reaction mixture, which
  3. waitto stand at room temperature for 16 hours
  4. filtrationThe precipitated crystals are filtered
  5. washwashed with 200 ml of water
  6. temperatureThe product is heated
  7. waitto boiling in 500 ml of methanol for 15 minutes
  8. filtrationfiltered
  9. washwashed with 400 ml of methanol
  10. dissolutiondissolved in hot dimethyl formamide
  11. customprecipitated
  12. additionby adding acetonitrile
  13. filtrationfiltered
  14. washwashed with acetonitrile

出典と根拠

ORDレコード
ord-5cb7f2412c014b9dafd0a467052e3d4b
出典データセット
uspto-grants-1989_05
特許番号
US04831029

反応ノート

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