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HCID 12620579、化合物 → 5-Methyl-4-oxo-4,5-dihydropyrano[3,2-b]indole-2-carboxylic acid

HRID 371657
ノート
印刷プレビュー

反応式

HRID 371657 の反応式
[CH3:1][N:2]1[C:10]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[C:4]2[O:11][C:12]([C:16]([O:18]CC)=[O:17])=[CH:13][C:14](=[O:15])[C:3]1=2>[OH-].[Na+]>[CH3:1][N:2]1[C:10]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[C:4]2[O:11][C:12]([C:16]([OH:18])=[O:17])=[CH:13][C:14](=[O:15])[C:3]1=2
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 12620579HCID 12620579、化合物

生成物 1

HCID 126205845-Methyl-4-oxo-4,5-dihydropyrano[3,2-b]indole-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

A mixture of 5.40g (0.020 mole) of ethyl 4,5-dihydro-5-methyl-4-oxopyrano [3,2-b]indole-2-carboxylate in 80ml of 1% aqueous sodium hydroxide was stirred at room temperature for 30 min. The nearly one-phase mixture was extracted twice with 50ml CH2Cl2 and the aqueous layer was cooled in ice and acidified with 4N HCl. The gelatinous yellow crude product was filtered, digested for a few minutes on a steam bath with 100ml hot water and then re-filtered. Recrystallization from ab. EtOH gave yellow needles of mpt. 280°-dec.

後処理

  1. extractionThe nearly one-phase mixture was extracted twice with 50ml CH2Cl2
temperature
the aqueous layer was cooled in ice
  • filtrationThe gelatinous yellow crude product was filtered
  • waitdigested for a few minutes on a steam bath with 100ml hot water
  • filtrationre-filtered
  • customRecrystallization from ab
  • customEtOH gave yellow needles of mpt
  • custom280°-dec
  • 出典と根拠

    ORDレコード
    ord-8b2e5e5a8fc94b3897dc2ce0dee69891
    出典データセット
    uspto-grants-1978_05
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04087443

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