m-Chloroperbenzoic acid → HCID 54215893, 화합물

HRID 892507노트

반응식

HRID 892507 반응식
[C:1]([C:4]1[CH:5]=[CH:6][C:7]2[O:12][C:11]([CH3:14])([CH3:13])[CH2:10][CH:9]([C:15]3[C:20]([CH3:21])=[CH:19][CH:18]=[CH:17][N:16]=3)[C:8]=2[CH:22]=1)(=[O:3])[CH3:2].ClC1C=CC=C(C(OO)=[O:31])C=1>ClCCl>[C:1]([C:4]1[CH:5]=[CH:6][C:7]2[O:12][C:11]([CH3:14])([CH3:13])[CH2:10][CH:9]([C:15]3[C:20]([CH3:21])=[CH:19][CH:18]=[CH:17][N+:16]=3[O-:31])[C:8]=2[CH:22]=1)(=[O:3])[CH3:2]

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 19895658HCID 19895658, 화합물

생성물 1

HCID 54215893HCID 54215893, 화합물수율 26.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

101 mg of 6-acetyl-3,4-dihydro-2,2-dimethyl-4-(3-methyl-2-pyridyl)-2H-1-benzopyran were dissolved in 5 ml of dichloromethane at room temperature and 91 mg of m-chloroperbenzoic acid were added. After 1 hour the mixture was washed in succession with sodium bisulphite solution, sodium bicarbonate solution and water. The organic extract was dried over sodium sulphate and evaporated to give an oil. This oil was triturated with t-butyl methyl ether to give a solid which, after recrystallization from ethyl acetate/t-butyl methyl ether, gave 28 mg of 2-(6-acetyl-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran-4-yl)-3-methylpyridine N-oxide of melting point 154°-156° C.

후처리

  1. washAfter 1 hour the mixture was washed in succession with sodium bisulphite solution, sodium bicarbonate solution and water
  2. extractionThe organic extract
  3. dry with materialwas dried over sodium sulphate
  4. customevaporated
  5. customto give an oil
  6. customThis oil was triturated with t-butyl methyl ether
  7. customto give a solid which
  8. customafter recrystallization from ethyl acetate/t-butyl methyl ether

출처 및 근거

ORD 기록
ord-1519956922e2441c9bf1fc295b54b7fc
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05118694

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