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6-amino-4-methyl-3,4-dihydro-2H-1,4-benzoxazin-3-one → HCID 59377423, 화합물

HRID 386662
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HRID 386662 반응식
[Br-:1].C([N+](C(C)(C)C)(C(C)(C)C)C(C)(C)C)(C)(C)C.[NH2:19][C:20]1[CH:21]=[CH:22][C:23]2[O:28][CH2:27][C:26](=[O:29])[N:25]([CH3:30])[C:24]=2[CH:31]=1>C(Cl)Cl.CO>[NH2:19][C:20]1[C:21]([Br:1])=[CH:22][C:23]2[O:28][CH2:27][C:26](=[O:29])[N:25]([CH3:30])[C:24]=2[CH:31]=1
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참가 물질

5

반응물 2

HCID 27644636-amino-4-methyl-3,4-dihydro-2H-1,4-benzoxazin-3-oneHCID 98185972-Propanaminium, N,N,N-tris(1,1-dimethylethyl)-2-methyl-, bromide

생성물 1

HCID 59377423HCID 59377423, 화합물수율 36%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

Tetra-tert-butyl ammonium bromide (6.77 g, 14.04 mmol) was added to a solution of 6-amino-4-methyl-4H-benzo[1,4]oxazin-3-one (2.5 g, 14.04 mmol) in methylene chloride (100 ml) and MeOH (50 ml). The mixture was stirred at room temperature for 20 minutes, then quenched with aqueous sodium bisulfite solution. The mixture was extracted with methylene chloride, and the combined organic extracts were dried over MgSO4, filtered, concentrated under reduced pressure and purified via column chromatography to give 1.30 g of 6-amino-7-bromo-4-methyl-4H-benzo[1,4]oxazin-3-one as a light yellow solid, 40%.

후처리

  1. customquenched with aqueous sodium bisulfite solution
  2. extractionThe mixture was extracted with methylene chloride
  3. dry with materialthe combined organic extracts were dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. custompurified via column chromatography

출처 및 근거

ORD 기록
ord-542b3f87ce0840ea9a032193ac67d623
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08372865B2

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