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Diethyl Ether → 6-(1-Oxo-2-morpholinoethyl)-3,4-dihydrocarbostyril monohydrochloride

HRID 2291185
ノート
印刷プレビュー

反応式

HRID 2291185 の反応式
[O:1]=[C:2]([C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][CH:14]=1)[NH:11][C:10](=[O:15])[CH2:9][CH2:8]2)[CH2:3][Cl:4].[NH:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1.CCOCC>O1CCOCC1>[ClH:4].[O:1]=[C:2]([C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][CH:14]=1)[NH:11][C:10](=[O:15])[CH2:9][CH2:8]2)[CH2:3][N:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 8083MorpholineHCID 49617906-(2-Chloroacetyl)-1,2,3,4-tetrahydroquinolin-2-one

生成物 1

HCID 202294546-(1-Oxo-2-morpholinoethyl)-3,4-dihydrocarbostyril monohydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

5.0 Grams of 6-(1-oxo-2-chloroethyl)-3,4-dihydrocarbostyril and 6.0 g of morpholine were dispersed in 120 ml of dioxane and stirred at 60°-70° C. for 12 hours. The reaction mixture was concentrated under a reduced pressure. The residue thus obtained was stirred with ether and the insoluble matter was collected by filtration and washed with water. Then the insoluble matter was dissolved in 80 ml of methanol and 10 ml of concentrated hydrochloric acid by heating and the solution was concentrated under a reduced pressure to dryness. The residue thus obtained was recrystallized from methanol-ether twice and obtained 5.9 g of 6-(1-oxo-2-morpholinoethyl)-3,4-dihydrocarbostyril monohydrochloride in colorless powdery product.

後処理

  1. concentrationThe reaction mixture was concentrated under a reduced pressure
  2. customThe residue thus obtained
  3. filtrationthe insoluble matter was collected by filtration
  4. washwashed with water
  5. dissolutionThen the insoluble matter was dissolved in 80 ml of methanol
  6. temperature10 ml of concentrated hydrochloric acid by heating
  7. concentrationthe solution was concentrated under a reduced pressure to dryness
  8. customThe residue thus obtained
  9. customwas recrystallized from methanol-ether twice

出典と根拠

ORDレコード
ord-d99857dc294642e48e5cb0d10df12c2d
出典データセット
uspto-grants-1986_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04619932

反応ノート

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