Aluminium lithium hydride → HCID 59497624、化合物

HRID 1747436ノート

反応式

HRID 1747436 の反応式
C[O:2][C:3]([C:5]1[C:13]2[N:9]([C:10]([CH3:15])=[C:11]([CH3:14])[CH:12]=2)[CH:8]=[CH:7][CH:6]=1)=O.[H-].[H-].[H-].[H-].[Li+].[Al+3]>CCOCC.C1COCC1>[CH3:14][C:11]1[CH:12]=[C:13]2[N:9]([C:10]=1[CH3:15])[CH:8]=[CH:7][CH:6]=[C:5]2[CH2:3][OH:2]

参加物

5

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 59497655HCID 59497655、化合物

生成物 1

HCID 59497624HCID 59497624、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of the 2,3-dimethyl-indolizine-8-carboxylic acid methyl ester (265 mg, 1.3 mmol) in ether (10 ml) was cooled to 0° C. and treated with LAH (1.0M in THF, 1.6 ml, 1.6 mmol, dropwise addition). After 3.5 h the reaction was quenched with sodium sulfate decahydrate (added in small portions until gas evolution ceased). The resulting mixture was stirred for 0.5 h and the precipitated solids were removed via filtration and washed with EtOAc. The combined filtrates were concentrated to give the product which was used without further purification.

後処理

  1. addition1.6 ml, 1.6 mmol, dropwise addition)
  2. customAfter 3.5 h the reaction was quenched with sodium sulfate decahydrate (added in small portions until gas evolution ceased)
  3. customthe precipitated solids were removed via filtration
  4. washwashed with EtOAc
  5. concentrationThe combined filtrates were concentrated
  6. customto give the product which
  7. customwas used without further purification

出典と根拠

ORDレコード
ord-8191f7235c714ddbb17dc534d885c7d8
出典データセット
uspto-grants-2015_10
特許番号
US09150556B2

反応ノート

読み込み中…