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Ammonium Acetate → HCID 13207875、化合物

HRID 918249
ノート
印刷プレビュー

反応式

HRID 918249 の反応式
[CH:1]12[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH2:3][CH:2]2[CH2:8][N:9]([C:16]1[CH:29]=[CH:28][C:27]([N+:30]([O-:32])=[O:31])=[CH:26][C:17]=1[C:18]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=O)[C:10](=[O:15])C(Cl)(Cl)Cl.C([O-])(=O)C.[NH4+:37]>C(O)(C)(C)C>[CH:1]12[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH2:3][CH:2]2[CH2:8][N:9]1[C:16]2[C:17](=[CH:26][C:27]([N+:30]([O-:32])=[O:31])=[CH:28][CH:29]=2)[C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[N:37][C:10]1=[O:15]
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 517165Ammonium Acetate2 回HCID 54358427HCID 54358427、化合物

生成物 1

HCID 13207875HCID 13207875、化合物

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

実験手順

To a solution of 2.5 g of 2-[ N-(2-norbornylmethyl)trichloroacetamido]-5-nitrobenzophenone in 50 ml of tert-butyl alcohol was added 2 g of ammonium acetate and the resulting mixture was heated under reflux for 7 hours. Then 2 g of ammonium acetate was added thereto and the reaction was continued for additional 8 hours. The solvent was removed under reduced pressure, and the residue was extracted with chloroform. The chloroform extract was washed with water, dried over anhydrous sodium sulfate, and evaporated to dryness. The residual oil was crystallized from a mixture of carbon tetrachloride and diethyl ether to give 1-(2-norbornylmethyl)-4-phenyl-6-nitro-2(1H)-quinazolinone, m.p. 160°C.

後処理

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 7 hours
  3. customThe solvent was removed under reduced pressure
  4. extractionthe residue was extracted with chloroform
  5. extractionThe chloroform extract
  6. washwas washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. customevaporated to dryness
  9. customThe residual oil was crystallized from a mixture of carbon tetrachloride and diethyl ether

出典と根拠

ORDレコード
ord-8f1e1147a88e41e3ae2d089d948350a5
出典データセット
uspto-grants-1976_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03970654

反応ノート

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