Nitric Acid → HCID 14771561, 화합물

HRID 329721노트

반응식

HRID 329721 반응식
[CH3:1][N:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[C:11]([C:12]([OH:14])=[O:13])[C:6]=2[O:5][CH2:4][C:3]1=[O:15].[N+:16]([O-])([OH:18])=[O:17]>S(=O)(=O)(O)O>[CH3:1][N:2]1[C:7]2[CH:8]=[C:9]([N+:16]([O-:18])=[O:17])[CH:10]=[C:11]([C:12]([OH:14])=[O:13])[C:6]=2[O:5][CH2:4][C:3]1=[O:15]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 14802113HCID 14802113, 화합물

생성물 1

HCID 14771561HCID 14771561, 화합물

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

To a solution of 85.5 g of 3,4-dihydro-4-methyl-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid in 222 ml of concentrated sulfuric acid with cooling to -8° C. is added dropwise with stirring a mixture of 20.7 ml of fuming nitric acid (d 1.50) and 20.7 ml of concentrated sulfuric acid at a temperature below 2° C. over about 30 minutes, and the solution further stirred under cooling. The resultant solution is poured into ice-cold water with stirring. The precipitated crystals are collected by filtration, washed with water and dried to give 99 g of 3,4-dihydro-4-methyl-6-nitro-3-oxo-2H-1,4-benzoxazine-8-carboxylic acid, melting at 256°-259° C. with decomposition.

후처리

  1. additionis added dropwise
  2. stirringthe solution further stirred
  3. temperatureunder cooling
  4. stirringwith stirring
  5. filtrationThe precipitated crystals are collected by filtration
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-1400f9909759411583e99233b5dad8fd
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04892872

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