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m-Chloroperbenzoic acid → HCID 9868455, 화합물

HRID 1835137
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HRID 1835137 반응식
[OH:1][CH2:2][CH2:3][CH2:4][S:5][C:6]1[N:7]([CH2:21][C:22]2[C:31]3[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=3)[CH:25]=[CH:24][CH:23]=2)[CH:8]=[C:9]2[C:14]([CH2:15][CH:16]([CH3:18])[CH3:17])=[N:13][N:12]([CH3:19])[C:11](=[O:20])[C:10]=12.ClC1C=C(C=CC=1)C(OO)=[O:37].C(=O)(O)[O-].[Na+].S(S([O-])=O)([O-])(=O)=O.[Na+].[Na+]>ClCCl>[OH:1][CH2:2][CH2:3][CH2:4][S:5]([C:6]1[N:7]([CH2:21][C:22]2[C:31]3[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=3)[CH:25]=[CH:24][CH:23]=2)[CH:8]=[C:9]2[C:14]([CH2:15][CH:16]([CH3:18])[CH3:17])=[N:13][N:12]([CH3:19])[C:11](=[O:20])[C:10]=12)=[O:37]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 656671Sodium PyrosulfiteHCID 5282542Mct1-IN-2

생성물 1

HCID 9868455HCID 9868455, 화합물수율 13.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2,6-Dihydro-7-[(3-hydroxypropyl)thio]-2-methyl-4-(2-methylpropyl)-6-(1-naphthalenylmethyl)-1H-pyrrolo[3,4-d]pyridazin-1-one (0.34 g) prepared as described in Example 3 above was dissolved in dichloromethane (7 ml) and 3-chloroperoxybenzoic acid (229 mg) was added. After 4 hours sodium bicarbonate (aqueous) and sodium metabisulfite (aqueous) were added and the mixture was extracted thrice with dichloromethane. The combined organic extracts were washed with brine, dried, filtered and evaporated. The residue was chromatographed eluting with ethyl acetate and then ethyl acetate:ethanol (19:1-9:1) to give 2 products. The more polar product was triturated with ether to give 2,6-Dihydro-7-[(3-hydroxypropyl)sulfinyl]-2-methyl-4(2-methylpropyl)-6-(1-naphthalenylmethyl)-1H-pyrrolo[3,4-d]pyridazin-1-one (A) (48 mg) whilst the less polar product was recrystallised from isohexane-ethyl acetate to give 2,6-dihydro-7-[(3-hydroxypropyl)sulfonyl]-2-methyl-4-(2-methylpropyl)-6-(1-naphthalenylmethyl)-1H-pyrrolo[3,4-d]pyridazin-1-one (B) (94 mg).

후처리

  1. extractionthe mixture was extracted thrice with dichloromethane
  2. washThe combined organic extracts were washed with brine
  3. customdried
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was chromatographed
  7. washeluting with ethyl acetate
  8. customethyl acetate:ethanol (19:1-9:1) to give 2 products
  9. customThe more polar product was triturated with ether

출처 및 근거

ORD 기록
ord-522006e159ae4fb19fb2cf9e350c715c
출처 데이터셋
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06770646B2

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