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Chloroform → 5-Amino-2-(4-chloro-2-methoxyphenyl)-4-methylthiazole

HRID 1498942
ノート
印刷プレビュー

反応式

HRID 1498942 の反応式
C(OC(=O)[NH:7][C:8]1[S:12][C:11]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=2[O:20][CH3:21])=[N:10][C:9]=1[CH3:22])(C)(C)C.Cl.O1CCOCC1.C(Cl)(Cl)Cl.C(=O)(O)[O-].[Na+]>CO>[NH2:7][C:8]1[S:12][C:11]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=2[O:20][CH3:21])=[N:10][C:9]=1[CH3:22]
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 6212ChloroformHCID 516892Sodium BicarbonateHCID 204431481,4-Dioxane hydrochlorideHCID 68641711[2-(4-Chloro-2-methoxyphenyl)-4-methylthiazol-5-yl]carbamic acid tert-butyl ester

生成物 1

HCID 686418935-Amino-2-(4-chloro-2-methoxyphenyl)-4-methylthiazole収率 65%

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

実験手順

In methanol (25 ml), [2-(4-chloro-2-methoxyphenyl)-4-methylthiazol-5-yl]carbamic acid tert-butyl ester (1.02 g, 2.87 mmol) prepared in the Step 28-1-1 was dissolved, and a 4-N hydrogen chloride-dioxane solution (25 ml) was added thereto. The mixture was stirred at a room temperature for 16 hours. Chloroform was added to the mixture, and the resulting mixture was neutralized with a saturated sodium bicarbonate solution. The resulting mixture was subjected to extraction with chloroform. The extract was dried over anhydrous magnesium sulfate and then concentrated. The concentrate was purified by silica gel column chromatography (chloroform:methanol=20:1) to give the title compound (474 mg, 65%) as a light-brown powder.

後処理

  1. dissolutionwas dissolved
  2. extractionThe resulting mixture was subjected to extraction with chloroform
  3. dry with materialThe extract was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customThe concentrate was purified by silica gel column chromatography (chloroform:methanol=20:1)

出典と根拠

ORDレコード
ord-2706ca54e753446ca5f1b61630640972
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09200008B2

反応ノート

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