Ammonium Hydroxide → HCID 20378679、化合物

HRID 2052109ノート

反応式

HRID 2052109 の反応式
[CH3:1][N:2]1[CH2:16][CH2:15][N:5]2[C:6]3[C:11]([NH:12][C:13](=O)[CH:4]2[CH2:3]1)=[CH:10][CH:9]=[CH:8][CH:7]=3.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[NH4+].C(O)(=O)/C=C/C(O)=O>CC(C)=O.O1CCCC1>[CH3:1][N:2]1[CH2:16][CH2:15][N:5]2[C:6]3[C:11]([NH:12][CH2:13][CH:4]2[CH2:3]1)=[CH:10][CH:9]=[CH:8][CH:7]=3

参加物

7

反応物 4

HCID 14923Ammonium HydroxideHCID 444972Fumaric Acid2 回HCID 20378670HCID 20378670、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 20378679HCID 20378679、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 7.1 g. of 2,3,4,4a-tetrahydro-3-methyl-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one, 3.5 g. of lithium aluminum hydride and 450 ml. of dry tetrahydrofuran is refluxed for 20 hours under a nitrogen atmosphere. The mixture is cooled and 20 ml. of concentrated ammonium hydroxide is carefully added. The mixture is filtered and the filter cake is washed with isopropanol. The filtrate is concentrated to give 5.7 g. of product as a viscous oil. A 3.5 g. portion is dissolved in acetone and treated with a saturated solution of fumaric acid in acetone. Filtration gives 3.3 g. of the product as the fumaric acid salt, m.p. 178°-188°. Recrystallization from isopropanol gives 2.1 g. of salt, m.p. 186°-188°.

後処理

  1. additionA mixture of 7.1 g
  2. temperatureThe mixture is cooled
  3. filtrationThe mixture is filtered
  4. washthe filter cake is washed with isopropanol
  5. concentrationThe filtrate is concentrated
  6. customto give 5.7 g
  7. filtrationFiltration
  8. customgives 3.3 g
  9. customRecrystallization from isopropanol
  10. customgives 2.1 g

出典と根拠

ORDレコード
ord-3846a93fb3c148a3a8d2639289a48174
出典データセット
uspto-grants-1980_01
特許番号
US04182872

反応ノート

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