Water → HCID 20570918、化合物

HRID 1577501ノート

反応式

HRID 1577501 の反応式
[CH3:1][N:2]([CH3:13])[C:3]([C:5]1[O:6][CH:7]=[CH:8][C:9]=1[CH:10]([CH3:12])[CH3:11])=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].O>O1CCCC1>[CH3:1][N:2]([CH3:13])[CH2:3][C:5]1[O:6][CH:7]=[CH:8][C:9]=1[CH:10]([CH3:11])[CH3:12]

参加物

5

反応物 3

HCID 962WaterHCID 20570904HCID 20570904、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 20570918HCID 20570918、化合物収率 63.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of N,N-dimethyl-3-(1-methylethyl)-2-furanecarboxamide (12 g) in dry tetrahydrofuran (250 ml) was treated with lithium aluminium hydride (4.2 g). After 1 hour water (6 ml) was added and the filtered solution evaporated in vacuo. The residue was dissolved in 1 M hydrochloric acid (100 ml) and the solution was washed with diethyl ether (100 ml). The aqueous phase was basified and extracted with diethyl ether (2×150 ml), which was dried over anhydrous sodium sulphate. The solvent was removed in vacuo to yield the title compound (7 g) as an oil.

後処理

  1. customthe filtered solution evaporated in vacuo
  2. dissolutionThe residue was dissolved in 1 M hydrochloric acid (100 ml)
  3. washthe solution was washed with diethyl ether (100 ml)
  4. extractionextracted with diethyl ether (2×150 ml), which
  5. dry with materialwas dried over anhydrous sodium sulphate
  6. customThe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-6b820ed1807f445c9f19370f85f509f3
出典データセット
uspto-grants-1981_09
特許番号
US04288443

反応ノート

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