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Ammonium Hydroxide → 6-nitro-2,2-dimethyl-3-aminomethyl-4-(2-oxo-1,2-dihydropyridin-1-yl)-2H-1-benzopyran

HRID 1655378
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HRID 1655378 반응식
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]2[O:12][C:11]([CH3:14])([CH3:13])[C:10]([CH2:15]Br)=[C:9]([N:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]3=[O:23])[C:8]=2[CH:24]=1)([O-:3])=[O:2].[OH-].[NH4+:26]>C(O)C>[N+:1]([C:4]1[CH:5]=[CH:6][C:7]2[O:12][C:11]([CH3:14])([CH3:13])[C:10]([CH2:15][NH2:26])=[C:9]([N:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]3=[O:23])[C:8]=2[CH:24]=1)([O-:3])=[O:2]
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참가 물질

4

반응물 2

HCID 14923Ammonium HydroxideHCID 193872966-nitro-2,2-dimethyl-3-bromomethyl-4-(2-oxo-1,2-dihydropyridin-1-yl)-2H-1-benzopyran

생성물 1

HCID 193870526-nitro-2,2-dimethyl-3-aminomethyl-4-(2-oxo-1,2-dihydropyridin-1-yl)-2H-1-benzopyran

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 6-nitro-2,2-dimethyl-3-bromomethyl-4-(2-oxo-1,2-dihydropyridin-1-yl)-2H-1-benzopyran (0.1 g, 0.255 mmol) in ethanol (2 ml) containing concentrated aqueous ammonium hydroxide solution (2 ml) was stirred at room temperature for four hours. The solvent was evaporated and the residue treated with ethanolic hydrochloric acid (2 ml) with heating. Crystallization was induced by addition of diethyl ether, giving 0.07 g of 6-nitro-2,2-dimethyl-3-aminomethyl-4-(2-oxo-1,2-dihydropyridin-1-yl)-2H-1-benzopyran as a hydrochloride salt, m.p. 231° C.

후처리

  1. customThe solvent was evaporated
  2. additionthe residue treated with ethanolic hydrochloric acid (2 ml)
  3. temperaturewith heating
  4. customCrystallization
  5. additionwas induced by addition of diethyl ether

출처 및 근거

ORD 기록
ord-0aed3ada77a64dbb9ef943821623a467
출처 데이터셋
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05250547

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