m-Chloroperbenzoic acid → HCID 53978841、化合物

HRID 892514ノート

反応式

HRID 892514 の反応式
[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

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 19895665HCID 19895665、化合物

生成物 1

HCID 53978841HCID 53978841、化合物収率 50.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7f37d2a9b50d42f98a304021cad0d524
出典データセット
uspto-grants-1992_06
特許番号
US05118694

反応ノート

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