Nitric Acid → 5-Fluoro-2-methyl-6-nitro-1,3-benzoxazole

HRID 9868

反応式

HRID 9868 の反応式
S(=O)(=O)(O)O.[F:6][C:7]1[CH:8]=[CH:9][C:10]2[O:14][C:13]([CH3:15])=[N:12][C:11]=2[CH:16]=1.O1C2C=CC=CC=2N=C1.[N+:26]([O-])([OH:28])=[O:27]>>[F:6][C:7]1[C:8]([N+:26]([O-:28])=[O:27])=[CH:9][C:10]2[O:14][C:13]([CH3:15])=[N:12][C:11]=2[CH:16]=1

参加物

5

反応物 4

HCID 944Nitric AcidHCID 1118Sulfuric Acid2 回HCID 9228BenzoxazoleHCID 27693505-Fluoro-2-methylbenzoxazole

生成物 1

HCID 136277005-Fluoro-2-methyl-6-nitro-1,3-benzoxazole

反応条件

温度
10 °C

実験手順

Concentrated sulfuric acid (60 mL) was stirred mechanically and cooled in an ice/water bath. To this was gradually added 5-fluoro-2-methylbenzoxazole (9), (20 g, 0.132 Moles), at such a rate that the temperature stayed at 15–20° C., over a 15–20 minute period. A solution of concentrated sulfuric acid (11 mL), and concentrated nitric acid (10 mL), was prepared and added drop by drop to the benzoxazole solution at such a rate that the temperature was maintained at approximately 10° C. When this acid solution had been added the cooling bath was removed and the mixture allowed to stir at room temperature for 1 hour. At the end of this period the solution was carefully poured onto ice with good stirring. Sufficient water was then added to get good mixing. The solid was filtered off, washed well with water and air-dried. Yield 16.0 g.

後処理

  1. temperaturecooled in an ice/water bath
  2. waitat such a rate that the temperature stayed at 15–20° C., over a 15–20 minute period
  3. additionWhen this acid solution had been added the cooling bath
  4. customwas removed
  5. additionAt the end of this period the solution was carefully poured onto ice with good stirring
  6. additionSufficient water was then added
  7. customto get good mixing
  8. filtrationThe solid was filtered off
  9. washwashed well with water
  10. customair-dried

出典と根拠

ORDレコード
ord-883bf0378f38498bbd32d6b2b6251006
出典データセット
uspto-grants-2006_08
特許番号
US07091361B2

関連ノート

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