Aluminium lithium hydride → HCID 68554248、化合物

HRID 2382117ノート

反応式

HRID 2382117 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[F:7][C:8]1[CH:9]=[CH:10][C:11]2[O:16][CH2:15][CH2:14][N:13]([N:17]=O)[C:12]=2[CH:19]=1>C1COCC1>[F:7][C:8]1[CH:9]=[CH:10][C:11]2[O:16][CH2:15][CH2:14][N:13]([NH2:17])[C:12]=2[CH:19]=1

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 866393826-Fluoro-4-nitroso-3,4-dihydro-2H-benzo[1,4]oxazine

生成物 1

HCID 68554248HCID 68554248、化合物収率 0.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

LiAlH4 in THF (1 M, 6.58 mL) is added to a solution of 6-fluoro-4-nitroso-3,4-dihydro-2H-benzo[1,4]oxazine (0.8 g) in THF (10 mL) at 00 C. and then stirred at rt overnight. The reaction mixture is quenched with a few drops of water followed by addition of EtOAc (10 mL). The solid is filtered off and washed with EtOAc (15 mL). The filtrate is concentrated in vacuo and the residue is purified by silica gel column chromatography eluting with 15% EtOAc in heptane to afford 6-fluoro-2,3-dihydro-benzo[1,4]oxazin-4-ylamine (0.44 mg).

後処理

  1. customThe reaction mixture is quenched with a few drops of water
  2. additionfollowed by addition of EtOAc (10 mL)
  3. filtrationThe solid is filtered off
  4. washwashed with EtOAc (15 mL)
  5. concentrationThe filtrate is concentrated in vacuo
  6. customthe residue is purified by silica gel column chromatography
  7. washeluting with 15% EtOAc in heptane

出典と根拠

ORDレコード
ord-5b9fab7643cb4a659da22f22c61899dd
出典データセット
uspto-grants-2012_09
特許番号
US08258130B2

反応ノート

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