Aluminium lithium hydride → HCID 20031090、化合物

HRID 232149ノート

反応式

HRID 232149 の反応式
C([O:3][C:4]([C:6]1[C:10]2[CH2:11][CH2:12][CH2:13][C:9]=2[N:8]([CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[N:7]=1)=O)C.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[CH2:14]([N:8]1[C:9]2[CH2:13][CH2:12][CH2:11][C:10]=2[C:6]([CH2:4][OH:3])=[N:7]1)[C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 54375111HCID 54375111、化合物

生成物 1

HCID 20031090HCID 20031090、化合物収率 1,065.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 1-benzyl-1,4,5,6-tetrahydro-3-cyclopentapyrazole carboxylic acid ethyl ester (6.0 g, 2.22 mmol) in THF (125 ml) was treated with lithium aluminum hydride (1.73 g, 44.4 mmol) and reacted at ambient temperature for 3.5 hours. Excess reagent was quenched with 10% aqueous THF (18 ml), 15% sodium hydroxide (5.4 ml) and water (5.4 ml). The mixture was diluted with ethyl acetate and filtered. The filtrate was washed with 5% brine solutions, dried, and evaporated to provide the title compound (5.40 g) as an oil.

後処理

  1. customreacted at ambient temperature for 3.5 hours
  2. customExcess reagent was quenched with 10% aqueous THF (18 ml), 15% sodium hydroxide (5.4 ml) and water (5.4 ml)
  3. additionThe mixture was diluted with ethyl acetate
  4. filtrationfiltered
  5. washThe filtrate was washed with 5% brine solutions
  6. customdried
  7. customevaporated

出典と根拠

ORDレコード
ord-ba1834a51b864f498493990d2345a5a1
出典データセット
uspto-grants-1989_07
特許番号
US04851425

反応ノート

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