Hydrochloric Acid → 1,2-Dihydro-9-hydroxy-7-(3-methyl-2-octyl)-4-oxo-4H-thieno[2,3-c][1]benzopyran

HRID 1282852ノート

反応式

HRID 1282852 の反応式
CO[C:3]([CH:5]1[C:9](=O)[CH2:8][S:7][CH2:6]1)=O.[CH3:11][CH:12]([CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[CH:13]([C:15]1[CH:16]=[C:17]([OH:22])C=[C:19]([CH:21]=1)[OH:20])[CH3:14].Cl.[CH2:29]([OH:31])C>>[OH:22][C:17]1[C:3]2[C:5]3[CH2:9][CH2:8][S:7][C:6]=3[C:29](=[O:31])[O:20][C:19]=2[CH:21]=[C:15]([CH:13]([CH:12]([CH3:11])[CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[CH3:14])[CH:16]=1

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 984243-Thiophenecarboxylic acid, tetrahydro-4-oxo-, methyl esterHCID 2581765-(3-Methyloctan-2-yl)benzene-1,3-diol

生成物 1

HCID 214339001,2-Dihydro-9-hydroxy-7-(3-methyl-2-octyl)-4-oxo-4H-thieno[2,3-c][1]benzopyran

実験手順

A solution of 20 g. (0.125 mole) of methyl-4-oxo-2,3,4,5-tetrahydrothiophene-3-carboxylate and 32 g. (0.135 mole of 5-(3-methyl-2-octyl)resorcinol in 200 ml. of absolute ethanol was cooled in an ice-salt bath and saturated with anhydrous hydrogen chloride. The reaction mixture was allowed to stand at room temperature for 72 hours and the solid which formed was removed by filtration. Recrystallization from ethanol gave 16 g. (37%) m.p. 165°-166°C. The structure was confirmed by infrared and nuclear magnetic resonance spectra.

後処理

  1. customthe solid which formed
  2. customwas removed by filtration
  3. customRecrystallization from ethanol
  4. customgave 16 g

出典と根拠

ORDレコード
ord-bd84788681894d568ae26b156b2bfe7a
出典データセット
uspto-grants-1976_08
特許番号
US03972880

反応ノート

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