Ammonium Hydroxide → HCID 20378679, 화합물

HRID 437949노트

반응식

HRID 437949 반응식
[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

참가 물질

7

반응물 4

HCID 14923Ammonium HydroxideHCID 444972Fumaric Acid2회HCID 20378670HCID 20378670, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 20378679HCID 20378679, 화합물

시약·촉매·용매 2

HCID 180Acetone용매2회HCID 8028Tetrahydrofuran용매

실험 절차

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° .

후처리

  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

출처 및 근거

ORD 기록
ord-750dd0422c6a4e77a9d8f864237df011
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04032639

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