Ammonia → HCID 54298002、化合物

HRID 2073394ノート

反応式

HRID 2073394 の反応式
[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

参加物

4

反応物 3

HCID 222AmmoniaHCID 1118Sulfuric AcidHCID 54516723HCID 54516723、化合物

生成物 1

HCID 54298002HCID 54298002、化合物

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-aba89d40a2414223a0f40d7ad4fe73a1
出典データセット
uspto-grants-1990_04
特許番号
US04916148

反応ノート

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