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Hydrochloric Acid → 3-[4-Cyano-3-nitrophenyl]-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione

HRID 430922
ノート
印刷プレビュー

反応式

HRID 430922 の反応式
C(=O)([O-])[O-].[K+].[K+].[C-:7]#[N:8].[K+].F[C:11]1[CH:16]=[CH:15][C:14]([N:17]2[C:22](=[O:23])[CH:21]=[C:20]([C:24]([F:27])([F:26])[F:25])[NH:19][C:18]2=[O:28])=[CH:13][C:12]=1[N+:29]([O-:31])=[O:30].Cl.C#N>CN(C)C=O.O>[C:7]([C:11]1[CH:16]=[CH:15][C:14]([N:17]2[C:22](=[O:23])[CH:21]=[C:20]([C:24]([F:27])([F:26])[F:25])[NH:19][C:18]2=[O:28])=[CH:13][C:12]=1[N+:29]([O-:31])=[O:30])#[N:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 768Hydrogen CyanideHCID 9032Potassium Cyanide2 回HCID 11430Potassium CarbonateHCID 153346693-[4-Fluoro-3-nitrophenyl]-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione

生成物 1

HCID 153346703-[4-Cyano-3-nitrophenyl]-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

Potassium carbonate (16.6 g) and potassium cyanide (7.8 g) were added to a solution of 3-[4-fluoro-3-nitrophenyl]-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione (31.9 g) in 250 ml of anhydrous N,N-dimethylformamide. The reaction mixture was subsequently stirred for a total of 45 hours at 75-80° C., with two further additions of potassium cyanide (in total 4.6 g) since the reaction had not proceeded completely. For working-up, water (250 ml) was added to the reaction mixture after it had cooled. The pH was subsequently brought to 2-3 by adding 60 ml of 1 N. hydrochloric acid. After nitrogen had been passed through the mixture for 4 hours to expel the hydrocyanic acid which had been liberated, the precipitate formed was separated off, washed with water and petroleum ether and dried. Yield: 17.0 g; m.p.: 135° C.

後処理

  1. temperaturehad cooled
  2. additionby adding 60 ml of 1 N
  3. customthe precipitate formed
  4. customwas separated off
  5. washwashed with water and petroleum ether
  6. customdried

出典と根拠

ORDレコード
ord-c742b1c5b30a4ee78aaff6c4abc16244
出典データセット
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06656884B2

反応ノート

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