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Aluminium lithium hydride → (2-Ethyl-1,3-thiazol-5-yl)methanol

HRID 2072388
ノート
印刷プレビュー

反応式

HRID 2072388 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([C:9]1[S:10][C:11]([C:14](OC)=[O:15])=[CH:12][N:13]=1)[CH3:8]>O1CCCC1>[CH2:7]([C:9]1[S:10][C:11]([CH2:14][OH:15])=[CH:12][N:13]=1)[CH3:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydride2 回HCID 21408257Methyl 2-ethyl-thiazole-5-carboxylate

生成物 1

HCID 21408258(2-Ethyl-1,3-thiazol-5-yl)methanol収率 94.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

2.4 g of mixed lithium aluminum hydride was added under nitrogen to a solution of 11.3 g of methyl 2-ethyl-thiazole-5-carboxylate in 100 ml of anhydrous tetrahydrofuran at 20 to 25° C and the mixture was refluxed for 1 1/2 hours. After cooling the mixture, excess lithium aluminum hydride was destroyed by the addition of ethyl acetate. The mixture was added to water and was vacuum filtered. The recovered precipitate was empasted with ethyl acetate and then with a methanol-methylene chlorine mixture. The filtrate was washed with water, dried and evaporated to dryness to obtan 9.5 g of an oil which was rectified under reduced pressure to obtain 8.9 g of 2-ethyl-thiazole-5-methanol with a boiling point of 78° C at 0.1 mm Hg.

後処理

  1. temperaturethe mixture was refluxed for 1 1/2 hours
  2. customwas destroyed by the addition of ethyl acetate
  3. additionThe mixture was added to water
  4. filtrationfiltered
  5. washThe filtrate was washed with water
  6. customdried
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-49c31ad84948443cb38705d0e2a7dc76
出典データセット
uspto-grants-1977_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04051249

反応ノート

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