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Pyridine → 2-isopropyl-2-methyl-5H-furo[2,3-b]imidazo[2',1':5,1]pyrrolo[3,4-e]pyridine-3(2H), 5-dione

HRID 1906111
ノート
印刷プレビュー

反応式

HRID 1906111 の反応式
[CH:1]([C:4]1([CH3:22])[C:8](=[O:9])[NH:7][C:6]([C:10]2[N:15]=[C:14]3[O:16][CH:17]=[CH:18][C:13]3=[CH:12][C:11]=2[C:19](O)=[O:20])=[N:5]1)([CH3:3])[CH3:2].C(OC(=O)C)(=O)C.N1C=CC=CC=1>C(COC)OC>[CH:1]([C:4]1([CH3:22])[C:8](=[O:9])[N:7]2[C:19](=[O:20])[C:11]3[CH:12]=[C:13]4[CH:18]=[CH:17][O:16][C:14]4=[N:15][C:10]=3[C:6]2=[N:5]1)([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 137524676-(4-Isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl)furo[2,3-b]pyridine-5-carboxylic acid

生成物 1

HCID 138496102-isopropyl-2-methyl-5H-furo[2,3-b]imidazo[2',1':5,1]pyrrolo[3,4-e]pyridine-3(2H), 5-dione収率 100.5%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

To a suspension of 6-(4-isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl)-furo[2,3-b]-pyridine-5-carboxylic acid (11.7 g, 0.039 mol) in 100 mL dimethoxyethane (DME) is added 7.3 mL acetic anhydride and 3.9 mL pyridine. After stirring 24 hours at room temperature, the solids are filtered and washed with ether and the mother liquor is concentrated by adding xylene to aid removal of pyridine. The residue is triturated with ether to obtain solids which are combined with the first crop to give 11.1 g (100%) of product. Recrystallization from 2:1 ethyl acetate-hexane gives an analytical sample mp 193°-205° C.

後処理

  1. filtrationthe solids are filtered
  2. washwashed with ether
  3. concentrationthe mother liquor is concentrated
  4. additionby adding xylene
  5. customremoval of pyridine
  6. customThe residue is triturated with ether
  7. customto obtain solids which

出典と根拠

ORDレコード
ord-dc6243e96c2c42ebb1e021f7d71db765
出典データセット
uspto-grants-1987_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04650514

反応ノート

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