Water → HCID 18408501、化合物

HRID 992985ノート

反応式

HRID 992985 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:13]2[S:14][CH:15]=[C:16]([C:18](OCC)=[O:19])[N:17]=2)[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[OH:19][CH2:18][C:16]1[N:17]=[C:13]([C:5]2[CH:4]=[C:3]([O:2][CH3:1])[C:8]([O:9][CH3:10])=[C:7]([O:11][CH3:12])[CH:6]=2)[S:14][CH:15]=1

参加物

6

反応物 4

HCID 962WaterHCID 24436Sodium SulfateHCID 18408534HCID 18408534、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 18408501HCID 18408501、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

Ethyl 2-(3,4,5-trimethoxyphenyl)thiazole-4-carboxylate (6.9 g) was dissolved in THF (100 mL), and to the solution lithium aluminum hydride (810 mg) was added under an argon atmosphere, and the mixture was stirred at 0° C. for 1 hour. After a small amount of water and then sodium sulfate were added to the reaction mixture, the reaction mixture was filtered through celite, and the filtrate was concentrated under reduced pressure. The resultant crude crystals were recrystallized from ethyl acetate-hexane to obtain the title compound.

後処理

  1. filtrationthe reaction mixture was filtered through celite
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe resultant crude crystals were recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-e86c20bb70d64800a1b1d552c7a60612
出典データセット
uspto-grants-2002_10
特許番号
US06472386B1

反応ノート

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