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Guanidine, 1,1-dimethyl-, sulfate → 4-Amino-2(-N,N-dimethylamino)-5-(2,3,5-trichlorophenyl)-6-trifluoromethyl pyrimidine

HRID 727039
ノート
印刷プレビュー

反応式

HRID 727039 の反応式
CC[O-].[Na+].S(O)(O)(=O)=O.[CH3:10][N:11]([CH3:15])[C:12]([NH2:14])=[NH:13].[Cl:16][C:17]1[C:22]([Cl:23])=[CH:21][C:20]([Cl:24])=[CH:19][C:18]=1[C:25](=[C:28](OC)[C:29]([F:32])([F:31])[F:30])[C:26]#[N:27]>CCO>[NH2:27][C:26]1[C:25]([C:18]2[CH:19]=[C:20]([Cl:24])[CH:21]=[C:22]([Cl:23])[C:17]=2[Cl:16])=[C:28]([C:29]([F:32])([F:31])[F:30])[N:14]=[C:12]([N:11]([CH3:15])[CH3:10])[N:13]=1
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 220673Guanidine, 1,1-dimethyl-, sulfateHCID 2723922Sodium ethoxideHCID 544228532-(2,3,5-Trichlorophenyl)-4,4,4-trifluoro-3-methoxybut-2-enonitrile

生成物 1

HCID 115238784-Amino-2(-N,N-dimethylamino)-5-(2,3,5-trichlorophenyl)-6-trifluoromethyl pyrimidine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To a solution of NaOEt (from 0.144 g of Na) in EtOH (12.5 ml) was added 1,1-dimethylguanidine sulphate (1.4 g), (Aldrich). The resulting white suspension was stirred at room temperature for 10 minutes. A solution of 2-(2,3,5-trichlorophenyl)-4,4,4-trifluoro-3-methoxybut-2-enonitrile (see Example 1.6) (0.85 g) in EtOH (2.5 ml) was added and the resulting mixture was stirred at reflux for 4.5 hours. After cooling, the suspension was filtered, and the filtrate was evaporated to dryness in vacuo. Chromatography on silica gel, eluting with CHCl3, gave the desired product, 0.61 g, mp. 124°-126° C.

後処理

  1. stirringthe resulting mixture was stirred
  2. temperatureat reflux for 4.5 hours
  3. temperatureAfter cooling
  4. filtrationthe suspension was filtered
  5. customthe filtrate was evaporated to dryness in vacuo
  6. washChromatography on silica gel, eluting with CHCl3

出典と根拠

ORDレコード
ord-838b56701bc446418b06392d63a11605
出典データセット
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05712276

反応ノート

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