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Dichloromethane → methyl 5-(3-pyrrolin-1-yl)-2-oxo-2H-[1,2,4]-oxadiazolo[2,3-a]pyrimidine-7-carbamate

HRID 26412
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HRID 26412 반응식
[N:1]1([C:6]2[N:11]=[C:10]([NH:12][C:13](OC)=[O:14])[N+:9]([O-:17])=[C:8]([NH:18][C:19]([O:21][CH3:22])=[O:20])[CH:7]=2)[CH2:5][CH:4]=[CH:3][CH2:2]1.C(Cl)Cl.[OH-].[Na+]>O>[N:1]1([C:6]2[CH:7]=[C:8]([NH:18][C:19]([O:21][CH3:22])=[O:20])[N:9]3[O:17][C:13](=[O:14])[N:12]=[C:10]3[N:11]=2)[CH2:5][CH:4]=[CH:3][CH2:2]1
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참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 178501987HCID 178501987, 화합물

생성물 1

HCID 20384865methyl 5-(3-pyrrolin-1-yl)-2-oxo-2H-[1,2,4]-oxadiazolo[2,3-a]pyrimidine-7-carbamate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

4.5 G. of dimethyl 6-(3-pyrrolin-1-yl)-2,4-pyrimidine-dicarbamate-3-oxide are suspended in a mixture of 200 ml. of methylene chloride and 200 ml. of water. The suspension is adjusted with concentrated sodium hydroxide to pH 12.5 and stirred at this pH for 3 hours. The two phases are then separated and the aqueous phase is adjusted to pH 3 with concentrated hydrochloric acid. The separated white precipitate is filtered off, pre-dried and recrystallized from a mixture of methylene chloride and methanol, there being obtained pure methyl 5-(3-pyrrolin-1-yl)-2-oxo-2H-[1,2,4]-oxadiazolo[2,3-a]pyrimidine-7-carbamate, having a melting point of 230°-234° C. (decomposition).

후처리

  1. customThe two phases are then separated
  2. filtrationThe separated white precipitate is filtered off
  3. custompre-dried
  4. customrecrystallized from a mixture of methylene chloride and methanol, there

출처 및 근거

ORD 기록
ord-a1761997908e46bfbaae4df6b5925058
출처 데이터셋
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04150131

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