Water → ((5-nitro-2-thiazolyl)thio)Pyrazine

HRID 46618

反応式

HRID 46618 の反応式
O.O.O.O.O.O.O.O.O.[S-2:10].[Na+].[Na+].Cl[C:14]1[CH:19]=[N:18][CH:17]=[CH:16][N:15]=1.Br[C:21]1[S:22][C:23]([N+:26]([O-:28])=[O:27])=[CH:24][N:25]=1.O>CN(C)C=O>[N+:26]([C:23]1[S:22][C:21]([S:10][C:14]2[CH:19]=[N:18][CH:17]=[CH:16][N:15]=2)=[N:25][CH:24]=1)([O-:28])=[O:27]

参加物

6

反応物 4

HCID 962WaterHCID 182112-Bromo-5-nitrothiazoleHCID 73277ChloropyrazineHCID 73972Sodium sulfide nonahydrate

生成物 1

HCID 20386480((5-nitro-2-thiazolyl)thio)Pyrazine収率 72%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
40 °C

実験手順

To a solution of 60.0 g (0.25 mol) of sodium sulfide nonahydrate in 500 ml of dimethyl formamide was gradually added 29 g (0.25 mol) of chloropyrazine in 100 ml of dimethyl formamide. The solution was stirred overnight at approximately 40° C. following which 52.5 g (0.25 mol) of 2-bromo-5-nitrothiazole was added as a solid. This reaction mixture was stirred at room temperature for 4 hours. After this period it was poured into water. The resulting precipitate was collected by suction filtration, washed with water and dried. The crude product was crystallized from methanol to yield 38 g (72% yield) of yellowish-gold crystals, m.p. 129°-130° C. A sample was subjected to elemental analysis. The results obtained were as follows:

後処理

  1. additionwas added as a solid
  2. stirringThis reaction mixture was stirred at room temperature for 4 hours
  3. filtrationThe resulting precipitate was collected by suction filtration
  4. washwashed with water
  5. customdried
  6. customThe crude product was crystallized from methanol
  7. customto yield 38 g (72% yield) of yellowish-gold crystals, m.p. 129°-130° C
  8. customThe results obtained

出典と根拠

ORDレコード
ord-d6a3df8b95524e459345095859e7e471
出典データセット
uspto-grants-1979_11
特許番号
US04174394

関連ノート

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