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Acetic Acid → 61001-18-1

HRID 616718
ノート
印刷プレビュー

反応式

HRID 616718 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:10]=[C:11]3[C:20]4[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=4)[CH:14]=[CH:13][N:12]3[CH:21]=2)=[CH:5][CH:4]=1.C(O)C.C(O)(=O)C>[Pd].[OH-].[NH4+]>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:10]=[C:11]3[C:20]4[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=4)[CH2:14][CH2:13][N:12]3[CH:21]=2)=[CH:5][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 176Acetic AcidHCID 702EthanolHCID 7460612-(4-Methoxyphenyl)imidazo[2,1-a]isoquinoline

生成物 1

HCID 1315607761001-18-1

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 14923Ammonium Hydroxide溶媒

実験手順

To a one liter autoclave are charged 7.1 g. of 2-(4-methoxyphenyl)imidazo[2,1-a]isoquinoline, 210 ml. of ethanol, 150 ml. of acetic acid and 0.55 g. of 10% palladium on charcoal. After flushing and filling the autoclave with hydrogen, the mixture is hydrogenated at 90° C. and 10 atmospheres for 3 hours. After absorption of 1.5 atmospheres of hydrogen gas, the autoclave is cooled and vented and 200 ml. of CHCl3 is added to the reaction mixture. The catalyst is filtered off, and the solution is evaporated to dryness, giving a solid residue which is suspended in 10% ammonium hydroxide, then extracted with dichloromethane. After drying over Na2SO4, the organic solvent is evaporated off and the residue is crystallized from ethanol giving 4.55 g. of the title product, which melts at 179°-81° C.

後処理

  1. additionTo a one liter autoclave are charged 7.1 g
  2. customAfter flushing
  3. customis hydrogenated at 90° C.
  4. customAfter absorption of 1.5 atmospheres of hydrogen gas
  5. temperaturethe autoclave is cooled
  6. additionof CHCl3 is added to the reaction mixture
  7. filtrationThe catalyst is filtered off
  8. customthe solution is evaporated to dryness
  9. customgiving a solid residue which
  10. extractionextracted with dichloromethane
  11. dry with materialAfter drying over Na2SO4
  12. customthe organic solvent is evaporated off
  13. customthe residue is crystallized from ethanol giving 4.55 g

出典と根拠

ORDレコード
ord-cfdf6ad783294052bf990d6e9b5e2dcc
出典データセット
uspto-grants-1978_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04075342

反応ノート

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