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5-Amino-4-chloro-3-ethylisothiazole → HCID 22742112、化合物

HRID 48173
ノート
印刷プレビュー

反応式

HRID 48173 の反応式
[NH2:1][C:2]1[S:6][N:5]=[C:4]([CH2:7][CH3:8])[C:3]=1[Cl:9].C[O-].[Na+].[CH3:13][CH:14]([CH3:31])[CH2:15][C:16]1[S:17][C:18]2[CH:24]=[CH:23][C:22]([CH:25]([CH3:30])[C:26](OC)=[O:27])=[CH:21][C:19]=2[N:20]=1>O1CCCC1.[Cl-].[NH4+]>[Cl:9][C:3]1[C:4]([CH2:7][CH3:8])=[N:5][S:6][C:2]=1[NH:1][C:26](=[O:27])[CH:25]([C:22]1[CH:23]=[CH:24][C:18]2[S:17][C:16]([CH2:15][CH:14]([CH3:13])[CH3:31])=[N:20][C:19]=2[CH:21]=1)[CH3:30]
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 3

HCID 98774685-Amino-4-chloro-3-ethylisothiazoleHCID 10942334Sodium MethoxideHCID 22742088Methyl 2-[2-(2-methylpropyl)benzothiazol-5-yl]propionate

生成物 1

HCID 22742112HCID 22742112、化合物収率 65%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回
HCID 25517
Ammonium Chloride
溶媒

実験手順

5-Amino-4-chloro-3-ethylisothiazole (0.81 g, 0.005 mol) was added to a suspension of sodium methoxide (0.56 g, 0.010 mol) in tetrahydrofuran (5 ml) and the mixture stirred at room temperature for 25 minutes. A solution of methyl 2-[2-(2-methylpropyl)benzothiazol-5-yl]propionate (1.15 g, 0.004 mol) in tetrahydrofuran (4 ml) was added dropwise and the mixture stirred at room temperature for 1½ hours. The mixture was diluted with saturated aqueous ammonium chloride solution and extracted with dichloromethane. The organic extract was dried over anhydrous magnesium sulfate, filtered and the filtrate evaporated in vacuo. Trituration with diethyl ether gave the desired product (1.06 g).

後処理

  1. stirringthe mixture stirred at room temperature for 1½ hours
  2. extractionextracted with dichloromethane
  3. extractionThe organic extract
  4. dry with materialwas dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customthe filtrate evaporated in vacuo

出典と根拠

ORDレコード
ord-6c19937bc9344f95a37626e2dfe904b9
出典データセット
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06703347B2

反応ノート

読み込み中…

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