Water → HCID 54516723、化合物

HRID 2073386ノート

反応式

HRID 2073386 の反応式
Br[CH2:2][C:3]1[CH:15]=[C:14]2[C:6]([CH:7]=[CH:8][C:9]3[O:10][C:11](=[O:18])[C:12]([CH3:17])([CH3:16])[C:13]=32)=[CH:5][C:4]=1[C:19]#[N:20].[NH:21]1[CH:25]=[N:24][CH:23]=[N:22]1.[Na].O>CN(C)C=O>[CH3:16][C:12]1([CH3:17])[C:11](=[O:18])[O:10][C:9]2[CH:8]=[CH:7][C:6]3[C:14]([C:13]1=2)=[CH:15][C:3]([CH2:2][N:21]1[CH:25]=[N:24][CH:23]=[N:22]1)=[C:4]([C:19]#[N:20])[CH:5]=3

参加物

5

反応物 3

HCID 962WaterHCID 19858052HCID 19858052、化合物HCID 454898221h-1,2,4-Triazole sodium salt

生成物 1

HCID 54516723HCID 54516723、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 8-bromomethyl-1,2-dihydro-1,1-dimethyl-2-oxonaphtho[2,1-b]furan-7-carbonitrile in N,N-dimethylformamide (3 ml) was treated with sodium 1,2,4-triazole (0.18 g) and the mixture was stirred at room temperature for 4 h, then treated with water (20 ml). The mixture was extracted twice with ethyl acetate and the combined extracts were dried and evaporated to dryness under reduced pressure. The residue was purified by flash chromatography using methanol:ethyl acetate, 1:99 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-carbonitrile, m.p. 198°-198° after recrystallisation from a mixture of ethyl acetate and cyclohexane.

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-0ba36d953b764eb2a1c30c098a990ba3
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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