Nitric Acid → Benzothiazole, 2-methyl-6-nitro-

HRID 389237ノート

反応式

HRID 389237 の反応式
[CH3:1][C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[N+:11]([O-])([OH:13])=[O:12]>S(=O)(=O)(O)O>[CH3:1][C:2]1[S:3][C:4]2[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:5]=2[N:6]=1

参加物

4

反応物 2

HCID 944Nitric AcidHCID 84462-Methylbenzothiazole

生成物 1

HCID 76250Benzothiazole, 2-methyl-6-nitro-

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

実験手順

2-Methylbenzothiazole (22 g) in conc. sulfuric acid (80 ml) was cooled to −5° C. A mixture of conc. sulfuric acid (12 ml) in conc. nitric acid (20 ml) was added so as to maintain the temperature below 5° C. (ca. 1.5 hours). After this time the mixture was allowed to warm to room temperature and the solution poured onto ice to give a yellow precipitate. The solid was removed by filtration and recrystallised from ethanol. After filtration the solid was washed with ethanol and dried in a vacuum oven to give 18 g of the desired product.

後処理

  1. additionwas added so as
  2. temperatureto maintain the temperature below 5° C. (ca. 1.5 hours)
  3. additionthe solution poured onto ice
  4. customto give a yellow precipitate
  5. customThe solid was removed by filtration
  6. customrecrystallised from ethanol
  7. filtrationAfter filtration the solid
  8. washwas washed with ethanol
  9. customdried in a vacuum oven

出典と根拠

ORDレコード
ord-7ec952db036a4857925fed474845cfc9
出典データセット
uspto-grants-2013_02
特許番号
US08378120B2

反応ノート

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