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Methyl iodide → Ethyl 7-formyl-6-methyl-2-(methylsulfanyl)pyrazolo[5,1-b][1,3]thiazole-3-carboxylate

HRID 41255
ノート
印刷プレビュー

反応式

HRID 41255 の反応式
[CH2:1]([O:3][C:4](=[O:15])[CH2:5][N:6]1[C:10](Cl)=[C:9]([CH:12]=[O:13])[C:8]([CH3:14])=[N:7]1)[CH3:2].[OH-].[K+].[C:18](=[S:20])=[S:19].[CH3:21]I>CS(C)=O>[CH:12]([C:9]1[C:8]([CH3:14])=[N:7][N:6]2[C:5]([C:4]([O:3][CH2:1][CH3:2])=[O:15])=[C:18]([S:20][CH3:21])[S:19][C:10]=12)=[O:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 6348Carbon DisulfideHCID 14797Potassium HydroxideHCID 737985ethyl 2-(5-chloro-4-formyl-3-methyl-1H-pyrazol-1-yl)acetate

生成物 1

HCID 3507588Ethyl 7-formyl-6-methyl-2-(methylsulfanyl)pyrazolo[5,1-b][1,3]thiazole-3-carboxylate

試薬・触媒・溶媒 1

HCID 679
Dimethyl Sulfoxide
溶媒

実験手順

To a mixture of ethyl(5-chloro-4-formyl-3-methyl-1H-pyrazol-1-yl)acetate (560 mg, 2.43 mmol), potassium hydroxide (495 mg, 7.5 mmol) and DMSO (9.72 mL) was added carbon disulfide (194 μL, 3.21 mmol), and the mixture was stirred at room temperature for 18 hours. To the reaction mixture, methyl iodide (182 μL, 2.92 mmol) was added, and the mixture was further stirred at room temperature for 8 hours. This reaction mixture was poured into ice water to yield a solid, and the obtained solid was filtered, and then washed with water and dried to obtain the title compound (346.1 mg, 1.22

後処理

  1. stirringthe mixture was further stirred at room temperature for 8 hours
  2. customto yield a solid
  3. filtrationthe obtained solid was filtered
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-4fc206117a124bfe8a8d7c0a53feda75
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08530504B2

反応ノート

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