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HCID 13935129、化合物 → 104628-27-5

HRID 580731
ノート
印刷プレビュー

反応式

HRID 580731 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:23]=[CH:24][CH:25]=1)[CH2:6][NH:7][C:8]1[C:9]2[C:14]([N:15]=[C:16]3[C:21]=1[C:20](=[O:22])[CH2:19][CH2:18][CH2:17]3)=[CH:13][CH:12]=[CH:11][CH:10]=2.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:23]=[CH:24][CH:25]=1)[CH2:6][NH:7][C:8]1[C:9]2[C:14]([N:15]=[C:16]3[C:21]=1[CH:20]([OH:22])[CH2:19][CH2:18][CH2:17]3)=[CH:13][CH:12]=[CH:11][CH:10]=2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 13935129HCID 13935129、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 3025617104628-27-5

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

3,4-Dihydro-9-(3-methoxybenzylamino)acridin-1(2H)-one (4.0 g) was dissolved in 75 ml of dry THF, the solution was chilled with ice-water, and 1M lithium aluminum hydride (6.5 ml) was added dropwise through a syringe. After 30 minutes TLC showed that the reaction was complete, so the reaction was quenched by the successive addition of 0.4 ml of water, 0.4 ml of 15% sodium hydroxide, and 1.2 ml of water. The inorganic salts were filtered off and the organic phase was evaporated to an oil. Trituration with ether gave a solid that was filtered off and then recrystallized from ether-pentane to give 2.2 g of analytically pure product, mp 123°-125° C.

後処理

  1. additionwas added dropwise through a syringe
  2. customwas quenched by the successive addition of 0.4 ml of water, 0.4 ml of 15% sodium hydroxide, and 1.2 ml of water
  3. filtrationThe inorganic salts were filtered off
  4. customthe organic phase was evaporated to an oil
  5. customTrituration with ether gave a solid
  6. filtrationthat was filtered off
  7. customrecrystallized from ether-pentane
  8. customto give 2.2 g of analytically pure product, mp 123°-125° C.

出典と根拠

ORDレコード
ord-21c0034c83a14be0b7a470b7e5200c10
出典データセット
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04754050

反応ノート

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