Ammonia → HCID 54298002, 화합물

HRID 2073394노트

반응식

HRID 2073394 반응식
[CH3:1][C:2]1([CH3:24])[C:6](=[O:7])[O:5][C:4]2[CH:8]=[CH:9][C:10]3[C:15]([C:3]1=2)=[CH:14][C:13]([CH2:16][N:17]1[CH:21]=[N:20][CH:19]=[N:18]1)=[C:12]([C:22]#[N:23])[CH:11]=3.S(=O)(=O)(O)[OH:26].N>>[CH3:1][C:2]1([CH3:24])[C:6](=[O:7])[O:5][C:4]2[CH:8]=[CH:9][C:10]3[C:15]([C:3]1=2)=[CH:14][C:13]([CH2:16][N:17]1[CH:21]=[N:20][CH:19]=[N:18]1)=[C:12]([C:22]([NH2:23])=[O:26])[CH:11]=3

참가 물질

4

반응물 3

HCID 222AmmoniaHCID 1118Sulfuric AcidHCID 54516723HCID 54516723, 화합물

생성물 1

HCID 54298002HCID 54298002, 화합물

실험 절차

A solution of 1,2-dihydro-1,1-dimethyl-2-oxo-8-(1H-1,2,4-triazol-1-ylmethyl)naphtho[2,1-b]furan-7-carbonitrile, (0.35 g) and concentrated sulphuric acid (2 ml) was kept at room temperature for 18 h. The mixture was treated with crushed ice and neutralised with concentrated aqueous ammonia, and the mixture was extracted twice with ethyl acetate. The combined extracts were dried and evaporated to dryness under reduced pressure, and the residue was purified by flash chromatography using methanol:dichloromethane, 1:14 v/v, as eluant, to give 1,2-dihydro-1,1-dimethyl-2-oxo-8-(1H-1,2,4-triazol-1-ylmethyl)naphtho[2,1-b]furan-7-carboxamide, m.p. 231°-232° after recrystallisation from a mixture of methanol and ethyl acetate.

후처리

  1. extractionthe mixture was extracted twice with ethyl acetate
  2. customThe combined extracts were dried
  3. customevaporated to dryness under reduced pressure
  4. customthe residue was purified by flash chromatography

출처 및 근거

ORD 기록
ord-aba89d40a2414223a0f40d7ad4fe73a1
출처 데이터셋
uspto-grants-1990_04
특허 번호
US04916148

반응 노트

불러오는 중…