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Sodium Hydroxide → HCID 70539013, 화합물

HRID 1981096
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HRID 1981096 반응식
COC([N:5]1[N:12](C(OC)=O)[CH:11]2[CH:6]1[CH:7]1[CH:17]([O:18]C(=O)C)[CH:10]2[CH:9]=[CH:8]1)=O.[OH-].[Na+].[O-]Cl.[Na+]>>[OH:18][CH:17]1[CH:10]2[CH:9]=[CH:8][CH:7]1[CH:6]1[CH:11]2[N:12]=[N:5]1
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참가 물질

4

반응물 3

HCID 14798Sodium HydroxideHCID 23665760Sodium HypochloriteHCID 545192933,4-Dimethoxycarbonyl-9-acetoxy-3,4-diazatricyclo[4,2,1,02,5]non-7-ene

생성물 1

HCID 70539013HCID 70539013, 화합물

실험 절차

92 parts of 3,4-dimethoxycarbonyl-9-acetoxy-3,4-diazatricyclo[4,2,1,02,5 ]non-7-ene and 570 parts of 20 percent strength aqueous NaOH were stirred for 3 hours at 70° C., after which 356 parts of 13 percent strength by weight aqueous NaOCl were added dropwise at 40° C. and stirring was continued for 1 hour at 40° C. The reaction mixture was extracted continuously for 12 hours with 300 parts of CH2Cl2, the organic phase was dried with MgSO4, treated with active charcoal and evaporated down, and the residue was digested with 200 parts of petroleum ether. 36.4 parts (86 mol %) of 9-hydroxy-3,4-diazatricyclo[4,2,1,02,5 ]nona-3,7-diene of melting point 128° C. (from cyclohexane) were obtained. ##STR13##

후처리

  1. extractionThe reaction mixture was extracted continuously for 12 hours with 300 parts of CH2Cl2
  2. dry with materialthe organic phase was dried with MgSO4
  3. additiontreated with active charcoal
  4. customevaporated down

출처 및 근거

ORD 기록
ord-933105ac88b0404f9501d668716844b9
출처 데이터셋
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04512795

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