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Water → 5-octyl-5-[N-(2-hydroxyethyl)piperazinyl]barbituric acid

HRID 993072
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HRID 993072 반응식
Br[C:2]1([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[C:7](=[O:8])[NH:6][C:5](=[O:9])[NH:4][C:3]1=[O:10].[OH:19][CH2:20][CH2:21][N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1.O>CS(C)=O>[CH2:11]([C:2]1([CH:23]2[CH2:24][NH:25][CH2:26][CH2:27][N:22]2[CH2:21][CH2:20][OH:19])[C:7](=[O:8])[NH:6][C:5](=[O:9])[NH:4][C:3]1=[O:10])[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 76771-(2-Hydroxyethyl)piperazineHCID 184088325-Bromo-5-octylbarbituric acid

생성물 1

HCID 537770275-octyl-5-[N-(2-hydroxyethyl)piperazinyl]barbituric acid

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a solution of 5-Bromo-5-octylbarbituric Acid (23.52 g) in 70 ml of dimethylsulfoxide, kept under nitrogen atmosphere and at a temperature of 5-10° C., is dropped N-(2-hydroxyethyl)piperazine (36.2 ml), then the mixture is stirred at room temperature for 2 hours 30 minutes. The reaction mixture is poured into water (1 l) under stirring and cooling with an ice bath. The white solid which separates is recovered by filtration, washed with water and dried under vacuum at 40° C. to give, after crystallization from ethanol (140 ml) 10.91 g of the product as a white solid, m.p. 183-184° C.

후처리

  1. customkept under nitrogen atmosphere and at a temperature of 5-10° C.
  2. stirringunder stirring
  3. temperaturecooling with an ice bath
  4. filtrationThe white solid which separates is recovered by filtration
  5. washwashed with water
  6. customdried under vacuum at 40° C.
  7. customto give
  8. customafter crystallization from ethanol (140 ml) 10.91 g of the product as a white solid, m.p. 183-184° C.

출처 및 근거

ORD 기록
ord-5c76a301bf2b433191ebb84bd8384674
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06472396B1

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