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Ammonia → 2-Naphthalenecarboxamide, 5,6-dihydro-7-(1H-imidazol-1-yl)-

HRID 745980
ノート
印刷プレビュー

反応式

HRID 745980 の反応式
[N:1]1([C:6]2[CH2:7][CH2:8][C:9]3[C:14]([CH:15]=2)=[CH:13][C:12]([C:16]([OH:18])=O)=[CH:11][CH:10]=3)[CH:5]=[CH:4][N:3]=[CH:2]1.[NH3:19]>CN(C=O)C>[N:1]1([C:6]2[CH2:7][CH2:8][C:9]3[C:14]([CH:15]=2)=[CH:13][C:12]([C:16](=[O:18])[NH2:19])=[CH:11][CH:10]=3)[CH:5]=[CH:4][N:3]=[CH:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 222AmmoniaHCID 56009Rolafagrel

生成物 1

HCID 30215672-Naphthalenecarboxamide, 5,6-dihydro-7-(1H-imidazol-1-yl)-

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a suspension of 1,2-dihydro-3-(1-imidazolyl)-6-carboxy-naphthalene (500 mg) in DMF (10 ml) SOCl2 (2 ml) was added. Cooling in an ice bath, NH3 was passed through the reaction mixture, with stirring, for 4 hours. The reaction mixture was allowed to stand for 12 hours. The ammonium salt was filtered off and Et2O was added giving a precipitate which was chromatographed on silica gel with CHCl3 :CH3OH-CH3COOH (45:5:2.5) as eluant; 350 mg of 1,2-dihydro-3-(1-imidazolyl)-6-carbamoyl-naphthalene were obtained.

後処理

  1. additionwas added
  2. temperatureCooling in an ice bath
  3. waitto stand for 12 hours
  4. filtrationThe ammonium salt was filtered off
  5. additionEt2O was added
  6. customgiving a precipitate which
  7. customwas chromatographed on silica gel with CHCl3

出典と根拠

ORDレコード
ord-01c39f10fd8e405e91d60c7f4b803f7a
出典データセット
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04602022

反応ノート

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