m-Chloroperbenzoic acid → HCID 53978841, 화합물

HRID 892514노트

반응식

HRID 892514 반응식
[CH3:1][C:2]1([CH3:22])[CH2:7][CH:6]([C:8]2[C:13]([CH3:14])=[CH:12][CH:11]=[CH:10][N:9]=2)[C:5]2[CH:15]=[C:16]([N+:19]([O-:21])=[O:20])[CH:17]=[CH:18][C:4]=2[O:3]1.ClC1C=CC=C(C(OO)=[O:31])C=1>ClCCl>[CH3:1][C:2]1([CH3:22])[CH2:7][CH:6]([C:8]2[C:13]([CH3:14])=[CH:12][CH:11]=[CH:10][N+:9]=2[O-:31])[C:5]2[CH:15]=[C:16]([N+:19]([O-:21])=[O:20])[CH:17]=[CH:18][C:4]=2[O:3]1

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 19895665HCID 19895665, 화합물

생성물 1

HCID 53978841HCID 53978841, 화합물수율 50.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

248 mg of 3.4-dihydro-2,2-dimethyl-4-(3-methyl-2-pyridyl)-6-nitro-2H-1-benzopyran were dissolved in 20 ml of dichloromethane at room temperature and 222 mg of m-chloroperbenzoic acid were added. After stirring at room temperature overnight the solution was washed in succession with sodium bisulphite solution, sodium bicarbonate solution and water. The organic phase was dried over sodium sulphate and evaporated. The resulting solid was triturated with diethyl ether, filtered off and recrystallized from acetonitrile to give 133 mg of 2-(3,4-dihydro-2,2-dimethyl-6-nitro-2H-1-benzopyran-4-yl)-3-methylpyridine N-oxide of melting point 218°-220° C.

후처리

  1. washwas washed in succession with sodium bisulphite solution, sodium bicarbonate solution and water
  2. dry with materialThe organic phase was dried over sodium sulphate
  3. customevaporated
  4. customThe resulting solid was triturated with diethyl ether
  5. filtrationfiltered off
  6. customrecrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-7f37d2a9b50d42f98a304021cad0d524
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05118694

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