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Bromine → Methyl 2-amino-4-methylbenzo[d]thiazole-5-carboxylate

HRID 1263407
ノート
印刷プレビュー

反応式

HRID 1263407 の反応式
[CH3:1][C:2]1[C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:6][CH:5]=[CH:4][C:3]=1[NH:12][C:13]([NH2:15])=[S:14].BrBr>ClC1C=CC=CC=1>[NH2:15][C:13]1[S:14][C:4]2[CH:5]=[CH:6][C:7]([C:8]([O:10][CH3:11])=[O:9])=[C:2]([CH3:1])[C:3]=2[N:12]=1
参加物反応条件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 24408BromineHCID 18616039N-(2-Methyl-3-methoxycarbonylphenyl)thiourea

生成物 1

HCID 22390084Methyl 2-amino-4-methylbenzo[d]thiazole-5-carboxylate

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒2 回

反応条件

温度
0 °C

実験手順

56 g of N-(2-methyl-3-methoxycarbonylphenyl)thiourea (0.25 mol) were dissolved in 2 l of chlorobenzene, and the mixture was cooled to 0° C. 40 g of bromine (0.25 mol) in 100 ml of chlorobenzene were then added dropwise. The reaction mixture was heated at 90° C. for 3 h, and the precipitate was filtered off with suction and washed with methylene chloride. The precipitate was then dissolved in ethyl acetate and extracted with sodium bicarbonate solution. After washing and drying, the product was obtained by stripping off the solvent. Yield: 43 g (80%).

後処理

  1. temperatureThe reaction mixture was heated at 90° C. for 3 h
  2. filtrationthe precipitate was filtered off with suction
  3. washwashed with methylene chloride
  4. dissolutionThe precipitate was then dissolved in ethyl acetate
  5. extractionextracted with sodium bicarbonate solution
  6. washAfter washing
  7. customdrying
  8. customthe product was obtained

出典と根拠

ORDレコード
ord-1457830cd9ea443bbca17272e72d3e21
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06541423B1

反応ノート

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