Ethanol → HCID 13293066、化合物

HRID 904817ノート

反応式

HRID 904817 の反応式
[C:1]([NH:9][CH:10]1[CH2:19][CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]1=[O:20])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3].C(O)C>C1COCC1>[CH2:1]([NH:9][C@@H:10]1[CH2:19][CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C@H:11]1[OH:20])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 702EthanolHCID 13293063N-(1-Oxo-1,2,3,4-tetrahydronaphthalen-2-yl)benzamideHCID 21226445Aluminium lithium hydride

生成物 1

HCID 13293066HCID 13293066、化合物収率 897.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 2-benzamido-3,4-dihydronaphthalen-1(2H)-one (3.0 g, 1.1 mmole) in THF (150 ml) was added dropwise to a suspension of LiAlH4 (2.0 g) in THF (50 ml). The reaction was heated at reflux for 2 hr and then cooled to room temperature. Enough ethanol was added to destroy excess LiAlH4 followed by 150 ml of Rochell's salt solution (20%). The resulting mixture was extracted with ethyl acetate, the ethyl acetate layer was washed with brine and dried over Na2SO4. Evaporation of the solvent afforded 2.5 g (88%) of the product, m.p. 110°-114° C. After recrystallization from cyclohexane it had m.p. 112°-115° C.

後処理

  1. temperatureThe reaction was heated
  2. temperatureat reflux for 2 hr
  3. customto destroy excess LiAlH4
  4. extractionThe resulting mixture was extracted with ethyl acetate
  5. washthe ethyl acetate layer was washed with brine
  6. dry with materialdried over Na2SO4
  7. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-f43725a652944e8fa58691821f871460
出典データセット
uspto-grants-1983_12
特許番号
US04420480

反応ノート

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