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Potassium sodium tartarate → (2-Ethyl-4-methyl-1,3-thiazol-5-yl)methanol

HRID 1058358
ノート
印刷プレビュー

反応式

HRID 1058358 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].C([O:9][C:10]([C:12]1[S:16][C:15]([CH2:17][CH3:18])=[N:14][C:13]=1[CH3:19])=O)C.C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[K+]>C(OCC)C>[CH2:17]([C:15]1[S:16][C:12]([CH2:10][OH:9])=[C:13]([CH3:19])[N:14]=1)[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 9855836Potassium sodium tartarateHCID 21226445Aluminium lithium hydrideHCID 23560693Ethyl 2-ethyl-4-methyl-1,3-thiazole-5-carboxylate

生成物 1

HCID 15093928(2-Ethyl-4-methyl-1,3-thiazol-5-yl)methanol収率 67%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Lithium aluminum hydride (800 mg, 21.2 mmol) was added to a solution of 2-ethyl-4-methylthiazole-5-carboxylic acid ethyl ester (Example 11; 1.63 g, 8.2 mmol) in diethyl ether (100 mL). The solution was allowed to stir at room temperature for 4 h and was then poured carefully into an aqueous potassium sodium tartrate solution (30% w/v; 200 mL). After the mixture was allowed to stir at room temperature for 1 h, the layers were separated and the aqueous layer was extracted with ethyl acetate (100 mL). The combined organic layers were washed with brine (200 mL), dried (MgSO4), filtered and concentrated under reduced pressure to give 2-ethyl-4-methylthiazole-5-methanol (860 mg, 67% yield) as a colorless oil.

後処理

  1. stirringto stir at room temperature for 1 h
  2. customthe layers were separated
  3. extractionthe aqueous layer was extracted with ethyl acetate (100 mL)
  4. washThe combined organic layers were washed with brine (200 mL)
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-d3c7a23f6c014e06b19e28e6d33b6078
出典データセット
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06515124B2

反応ノート

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