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9-amino-3,4-dihydro-6-fluoroacridin-1(2H)-one → 1-Acridinol, 1,2,3,4-tetrahydro-9-amino-6-fluoro-

HRID 1904720
ノート
印刷プレビュー

反応式

HRID 1904720 の反応式
[NH2:1][C:2]1[C:3]2[C:8]([N:9]=[C:10]3[C:15]=1[C:14](=[O:16])[CH2:13][CH2:12][CH2:11]3)=[CH:7][C:6]([F:17])=[CH:5][CH:4]=2.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[NH2:1][C:2]1[C:3]2[C:8]([N:9]=[C:10]3[C:15]=1[CH:14]([OH:16])[CH2:13][CH2:12][CH2:11]3)=[CH:7][C:6]([F:17])=[CH:5][CH:4]=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 139351199-amino-3,4-dihydro-6-fluoroacridin-1(2H)-oneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 30256071-Acridinol, 1,2,3,4-tetrahydro-9-amino-6-fluoro-収率 99.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a cooled suspension of 5.0 g of 9-amino-3,4-dihydro-6-fluoroacridin-1(2H)-one in 85 ml of tetrahydrofuran was added 22 ml of 1M solution of lithium aluminum hydride in tetrahydrofuran. This was stirred for 1 hour and then quenched with 8 ml of saturated ammonium chloride solution. The inorganics were filtered and rinsed with ethyl acetate, and the combined organics were dried over anhydrous magnesium sulfate. This was filtered and concentrated to obtain 5.0 g of powder, mp 203°-206° C. d. This was recrystallized from tetrahydrofuran/hexane to obtain 3.95 g of an analytically pure powder, mp 207°-209° C. d.

後処理

  1. customquenched with 8 ml of saturated ammonium chloride solution
  2. filtrationThe inorganics were filtered
  3. washrinsed with ethyl acetate
  4. dry with materialthe combined organics were dried over anhydrous magnesium sulfate
  5. filtrationThis was filtered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-1de7ebc062f84c5c8d28dba0aa923675
出典データセット
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04839364

反応ノート

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