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Water → (2-chloro-4-pyrimidinyl)(3-methyl-1,3-benzothiazol-2(3H)-ylidene)ethanenitrile

HRID 854264
ノート
印刷プレビュー

反応式

HRID 854264 の反応式
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[CH:10]([C:13]1[CH:18]=[CH:17][N:16]=[C:15]([Cl:19])[N:14]=1)[C:11]#[N:12].[C:20]([O-])([O-])=O.[K+].[K+].CI.O>CS(C)=O>[Cl:19][C:15]1[N:14]=[C:13]([C:10](=[C:2]2[N:3]([CH3:20])[C:4]3[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=3[S:1]2)[C:11]#[N:12])[CH:18]=[CH:17][N:16]=1
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 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 3952292-(Benzo[d]thiazol-2-yl)-2-(2-chloropyrimidin-4-yl)acetonitrile

生成物 1

HCID 72806198(2-chloro-4-pyrimidinyl)(3-methyl-1,3-benzothiazol-2(3H)-ylidene)ethanenitrile収率 5%

試薬・触媒・溶媒 1

HCID 679
Dimethyl Sulfoxide
溶媒

実験手順

To a solution of 1 (0.1 g, 0.35 mmol) in dry DMSO was added dry K2CO3 then methyl iodide and the suspension was shaken at rt. for 2 days. The precipitate formed by addition of water was filtered off then washed with water until neutral pH. The crude residue, dried under vacuum at 40° C., was triturated in warm acetonitrile, filtered off then dried under vacuum at 40° C., affording 5.6 mg (5%) of the title compound as a yellow powder.

後処理

  1. filtrationwas filtered off
  2. washthen washed with water until neutral pH
  3. dry with materialThe crude residue, dried under vacuum at 40° C.
  4. customwas triturated in warm acetonitrile
  5. filtrationfiltered off
  6. customthen dried under vacuum at 40° C.

出典と根拠

ORDレコード
ord-2c2c8c3e997646b4bb045e10cbeefc6e
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07259162B2

反応ノート

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