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Water → HCID 135995202, 화합물

HRID 1925020
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HRID 1925020 반응식
[CH3:1][C:2]1[N:3]=[C:4]([C:8]2[C:9](=[O:15])[NH:10][C:11](=[O:14])[NH:12][CH:13]=2)[S:5][C:6]=1[CH3:7].[C:16](Cl)(=[O:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.O>N1C=CC=CC=1>[CH3:1][C:2]1[N:3]=[C:4]([C:8]2[C:9](=[O:15])[N:10]([C:16]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)=[O:23])[C:11](=[O:14])[NH:12][CH:13]=2)[S:5][C:6]=1[CH3:7]
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참가 물질

5

반응물 3

HCID 962WaterHCID 7412Benzoyl chlorideHCID 135995200HCID 135995200, 화합물

생성물 1

HCID 135995202HCID 135995202, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매2회

실험 절차

(5-(4,5-dimethyl-1,3-thiazol-2-yl)-2,4(1H,3H)-pyrimidinedione) (Prep 15, 100 mg) suspended in Pyridine (2 mL) was slowly added to a stirring solution of benzoyl chloride (0.156 ml, 1.344 mmol) in Pyridine (1 mL) under nitrogen atmosphere. The resulting yellow solution was stirred at rt for 5.5 hours. Water was added (3 mL) and the mixture was extracted with EtOAc (10 mL). The organic was washed with NH4Cl saturated aqueous solution (2×2 mL) dried (Na2SO4, vacuo) to afford 340 mg of a yellowish solid that was dissolved in EtOAc (30 mL) and washed with NaHCO3 aqueous saturated solution. The organic was dried (Na2SO4, vacuo) to afford the title compound as a yellowish solid (180 mg)

후처리

  1. extractionthe mixture was extracted with EtOAc (10 mL)
  2. washThe organic was washed with NH4Cl saturated aqueous solution (2×2 mL)
  3. dry with materialdried (Na2SO4, vacuo)

출처 및 근거

ORD 기록
ord-4a0815e670374299a10de0c60520916a
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08178549B2

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