HCID 13935130、化合物 → 104628-28-6

HRID 580732ノート

反応式

HRID 580732 の反応式
[CH3:1][O:2][C:3]1[CH:25]=[CH:24][C:6]([CH2:7][NH:8][C:9]2[C:10]3[C:15]([N:16]=[C:17]4[C:22]=2[C:21](=[O:23])[CH2:20][CH2:19][CH2:18]4)=[CH:14][CH:13]=[CH:12][CH:11]=3)=[CH:5][CH:4]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:7][NH:8][C:9]2[C:10]3[C:15]([N:16]=[C:17]4[C:22]=2[CH:21]([OH:23])[CH2:20][CH2:19][CH2:18]4)=[CH:14][CH:13]=[CH:12][CH:11]=3)=[CH:24][CH:25]=1

参加物

4

反応物 2

HCID 13935130HCID 13935130、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 3025618104628-28-6

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

3,4-Dihydro-9-(4-methoxybenzylamino)acridin-1(2H)-one (4.25 g) was dissolved in 75 ml of dry THF and chilled with ice-water. 1M lithium aluminum hydride in THF (7.0 ml) was then added dropwise. After 15 minutes the reaction was quenched by the sequential dropwise addition of 0.4 ml of water, 0.4 ml of 15% sodium hydride and 1.2 ml of water. The inorganic salts were filtered off, the solvents were evaporated, and the residue recrystallized from dichloromethane-ether to give 3.0 g of analytically pure product, mp 163°-165° C.

後処理

  1. customAfter 15 minutes the reaction was quenched by the sequential dropwise addition of 0.4 ml of water, 0.4 ml of 15% sodium hydride and 1.2 ml of water
  2. filtrationThe inorganic salts were filtered off
  3. customthe solvents were evaporated
  4. customthe residue recrystallized from dichloromethane-ether
  5. customto give 3.0 g of analytically pure product, mp 163°-165° C.

出典と根拠

ORDレコード
ord-20893bc9e9654c5caddd4d8d0fb575f7
出典データセット
uspto-grants-1988_06
特許番号
US04754050

反応ノート

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