6-Ethoxycarbonylamino-1-methyl-3,4-dihydroisoquinoline → 6-Ethoxycarbonylamino-1-methylisoquinoline

HRID 1173129ノート

反応式

HRID 1173129 の反応式
[CH2:1]([O:3][C:4]([NH:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[C:13]([CH3:17])=[N:12][CH2:11][CH2:10]2)=[O:5])[CH3:2]>[C].[Pd].CC1C=CC(C(C)C)=CC=1>[CH2:1]([O:3][C:4]([NH:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[C:13]([CH3:17])=[N:12][CH:11]=[CH:10]2)=[O:5])[CH3:2]

参加物

4

反応物 1

HCID 226741196-Ethoxycarbonylamino-1-methyl-3,4-dihydroisoquinoline

生成物 1

HCID 226741466-Ethoxycarbonylamino-1-methylisoquinoline収率 69%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 7463P-Cymene溶媒

反応条件

温度
195 °C

実験手順

p-Cymene (100 ml) and palladium carbon (0.9 g) were added to 6-ethoxycarbonylamino-1-methyl-3,4-dihydroisoquinoline, followed by heating under stirring at 195° C. for one hour in a nitrogen atmosphere. The catalyst was filtered off and washed with ethanol, and then the filtrate was partially evaporated. After extracting with 1N hydrochloric acid, the extract was basified with potassium carbonate and then extracted with ethyl acetate. The extract was washed with brine and dried over anhydrous magnesium sulfate anhydride. The solvent was evaporated, to give the title compound (0.629 g, 69%, 2 steps) as pale yellow crystals.

後処理

  1. temperatureby heating
  2. filtrationThe catalyst was filtered off
  3. washwashed with ethanol
  4. customthe filtrate was partially evaporated
  5. extractionAfter extracting with 1N hydrochloric acid
  6. extractionextracted with ethyl acetate
  7. washThe extract was washed with brine
  8. dry with materialdried over anhydrous magnesium sulfate anhydride
  9. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-fcfe666d5bc0439eb79fc1e8b0f2baf6
出典データセット
uspto-grants-2010_11
特許番号
US07834049B2

反応ノート

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