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

HRID 636346

반응식

HRID 636346 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8]([CH3:10])=[N:7][C:6]=2[CH:11]=1.[N+:12]([O-])([OH:14])=[O:13].O1C2C=CC=CC=2N=C1>S(=O)(=O)(O)O>[Cl:1][C:2]1[C:3]([N+:12]([O-:14])=[O:13])=[CH:4][C:5]2[O:9][C:8]([CH3:10])=[N:7][C:6]=2[CH:11]=1

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 9228BenzoxazoleHCID 295105-Chloro-2-methylbenzoxazole

생성물 1

HCID 27644555-Chloro-2-methyl-6-nitro-1,3-benzoxazole

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

반응 조건

온도
20 °C

실험 절차

Concentrated sulfuric acid (150 mL) was stirred mechanically and cooled in an ice/water bath. To this was gradually added 5-chloro-2-methylbenzoxazole (1), (75 g, 0.45 Moles) at such a rate that the temperature stayed at 30° C., over a 15-20 minute period. A solution of concentrated sulfuric acid (40 mL), and concentrated nitric acid (32 mL), was prepared and added drop by drop to the benzoxazole solution at such a rate that the temperature was maintained at approximately 20° 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 followed by methanol and finally air dried. Yield 90.6 g.

후처리

  1. temperaturecooled in an ice/water bath
  2. additionWhen this acid solution had been added the cooling bath
  3. customwas removed
  4. additionAt the end of this period the solution was carefully poured onto ice with good stirring
  5. additionSufficient water was then added
  6. customto get good mixing
  7. filtrationThe solid was filtered off
  8. washwashed well with water
  9. customdried

출처 및 근거

ORD 기록
ord-fc7999aeaecd49dfb3f6eebcbeaa0bbe
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06194132B1

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