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HCID 18712270、化合物 → HCID 62402682、化合物

HRID 1050720
ノート
印刷プレビュー

反応式

HRID 1050720 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([NH:9][C:10]([C:12]1[S:16][C:15]([CH3:17])=[N:14][C:13]=1[CH3:18])=O)[CH3:8]>O1CCCC1>[CH3:17][C:15]1[S:16][C:12]([CH2:10][NH:9][CH2:7][CH3:8])=[C:13]([CH3:18])[N:14]=1
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 18712270HCID 18712270、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 62402682HCID 62402682、化合物収率 72.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

0.8 g of lithium aluminum hydride and 20 mL of tetrahydrofuran were added in a 150 mL of single-neck flask equipped with a magnetic stirrer. After stirred for 0.5 to 1.0 hour under ice bath cooling, 1.5 g of N-ethyl-2,4-dimethylthiazole-5-carboxamide in 10 mL of tetrahydrofuran solution are added dropwise, and reacted at the same temperature for 0.5 to 10 hours, and then for 1 to 2 hours at room temperature. The reaction mixture was then extracted with ethyl acetate, the organic layer was separated while the aqueous layer was extracted with ethyl acetate twice. The organic phases were combined, and dried over anhydrous sodium sulfate after washed with an iced aqueous sodium chloride solution twice, then remove the solvent under reduced pressure to obtain 1.0 g of 2,4-dimethyl-5-ethylaminomethylthiazole which was used in the next step directly without purification.

後処理

  1. customequipped with a magnetic stirrer
  2. temperaturecooling
  3. customreacted at the same temperature for 0.5 to 10 hours
  4. waitfor 1 to 2 hours at room temperature
  5. extractionThe reaction mixture was then extracted with ethyl acetate
  6. customthe organic layer was separated while the aqueous layer
  7. extractionwas extracted with ethyl acetate twice
  8. dry with materialdried over anhydrous sodium sulfate
  9. washafter washed with an iced aqueous sodium chloride solution twice
  10. customremove the solvent under reduced pressure

出典と根拠

ORDレコード
ord-dab41ea18a4f4b09b7a67c6010d45e7c
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09386769B2

反応ノート

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