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Bromine → 5,7-dimethoxy-2-[(2-methoxycarbonylbenzyl)sulfonyl]imino-2H-[1,2,4]-thiadiazolo[2,3-a]pyrimidine

HRID 330454
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HRID 330454 반응식
[CH3:1][O:2][C:3]([C:5]1[CH:28]=[CH:27][CH:26]=[CH:25][C:6]=1[CH2:7][S:8]([NH:11][C:12]([NH:14][C:15]1[N:20]=[C:19]([O:21][CH3:22])[CH:18]=[C:17]([O:23][CH3:24])[N:16]=1)=[S:13])(=[O:10])=[O:9])=[O:4].BrBr>N1C=CC=CC=1>[CH3:24][O:23][C:17]1[CH:18]=[C:19]([O:21][CH3:22])[N:20]2[S:13][C:12](=[N:11][S:8]([CH2:7][C:6]3[CH:25]=[CH:26][CH:27]=[CH:28][C:5]=3[C:3]([O:2][CH3:1])=[O:4])(=[O:10])=[O:9])[N:14]=[C:15]2[N:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24408BromineHCID 14275714N-(2-Methoxycarbonylbenzyl)sulfonyl-N'-(4,6-dimethoxy-2-pyrimidinyl) thiourea

생성물 1

HCID 536931185,7-dimethoxy-2-[(2-methoxycarbonylbenzyl)sulfonyl]imino-2H-[1,2,4]-thiadiazolo[2,3-a]pyrimidine수율 78.4%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

N-(2-Methoxycarbonylbenzyl)sulfonyl-N'-(4,6-dimethoxy-2-pyrimidinyl) thiourea (1.0 g) is dissolved in 15 ml of pyridine and cooled to -10°~-5° C., to which 0.4 g of bromine is dropwise added. After stirring for 1.5 hours at the same temperature, the reaction mixture is poured into 100 ml of ice water and the white crystals are collected by filtration. The product is washed with water, dried and washed with hot acetonitrile to give 0.78 g of the title compound as white powdery crystals. mp 153°~154° C.

후처리

  1. additionis dropwise added
  2. filtrationthe white crystals are collected by filtration
  3. washThe product is washed with water
  4. customdried
  5. washwashed with hot acetonitrile

출처 및 근거

ORD 기록
ord-1a07ee0a836844969513b249e1efca91
출처 데이터셋
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04897105

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