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

HRID 46618

반응식

HRID 46618 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

반응 조건

온도
40 °C

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-d6a3df8b95524e459345095859e7e471
출처 데이터셋
uspto-grants-1979_11
특허 번호
US04174394

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