Aluminium lithium hydride → 2-(Methylamino)-4-(1-naphthyloxy)-1-butanol

HRID 1111687ノート

反応式

HRID 1111687 の反応式
[CH:1]([NH:3][CH:4]([CH2:7][CH2:8][O:9][C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH:13]=[CH:12][CH:11]=1)[CH2:5][OH:6])=O.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[CH3:1][NH:3][CH:4]([CH2:7][CH2:8][O:9][C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH:13]=[CH:12][CH:11]=1)[CH2:5][OH:6]

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 227550192-(Formylamino)-4-(1-naphthyloxy)butanol

生成物 1

HCID 203721512-(Methylamino)-4-(1-naphthyloxy)-1-butanol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
45 °C

実験手順

A solution of 2-(formylamino)-4-(1-naphthyloxy)butanol (7.1 g), prepared as described in Example 3, in dry THF (150 ml) is added dropwise to a suspension of LiAlH4 (5.0 g) in THF (150 ml). The mixture is heated at 45° C. for 3 hours and cooled. Excess LiAlH4 is destroyed by the careful addition of THF/water (9:1). The mixture is filtered through diatomaceous earth (Celite). The filtrate is dried and evaporated. The residue is crystallized from diethyl ether to give the title compound, γmaxCHCl3 3650, 3352, 1595 and 1580 cm-1.

後処理

  1. temperaturecooled
  2. customExcess LiAlH4 is destroyed by the careful addition of THF/water (9:1)
  3. filtrationThe mixture is filtered through diatomaceous earth (Celite)
  4. customThe filtrate is dried
  5. customevaporated
  6. customThe residue is crystallized from diethyl ether

出典と根拠

ORDレコード
ord-cef6e05c04b24ab7b332bd56258996a1
出典データセット
uspto-grants-1978_10
特許番号
US04118511

反応ノート

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