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Sodium → 3,4-dihydro-2H-[1,3]oxazino[3,2-a]benzimidazole

HRID 46866
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HRID 46866 반응식
[Na].CS(O)(=O)=O.O[CH2:8][CH2:9][CH2:10][N:11]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[NH:13][C:12]1=[O:20]>C(O)C>[O:20]1[C:12]2=[N:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[N:11]2[CH2:10][CH2:9][CH2:8]1
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참가 물질

4

반응물 2

HCID 5360545SodiumHCID 867353601,3-dihydro-1-(3-hydroxypropyl)-2H-benzimidazol-2-one methanesulfonate

생성물 1

HCID 110951143,4-dihydro-2H-[1,3]oxazino[3,2-a]benzimidazole

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 0.5 parts of sodium in 40 parts of absolute ethanol are added in the cold 5.4 parts of 1,3-dihydro-1-(3-hydroxypropyl)-2H-benzimidazol-2-one methanesulfonate. The whole is stirred until all solid enters solution. The solution is further stirred and refluxed for 2 hours. After cooling the reaction mixture is filtered from some inorganic matter and the filtrate is evaporated. The residue is dissolved in 80 parts of methylbenzene, boiled with activated charcoal, filtered and the filtrate is evaporated again. The solid residue is washed with cold methylbenzene and crystallized from 16 parts of methylbenzene, yielding 2.6 parts of 3,4-dihydro-2H-[1,3]oxazino[3,2-a]benzimidazole; mp. 116.5°-118.5° C.

후처리

  1. stirringThe solution is further stirred
  2. temperaturerefluxed for 2 hours
  3. temperatureAfter cooling the reaction mixture
  4. filtrationis filtered from some inorganic matter
  5. customthe filtrate is evaporated
  6. dissolutionThe residue is dissolved in 80 parts of methylbenzene
  7. filtrationfiltered
  8. customthe filtrate is evaporated again
  9. washThe solid residue is washed with cold methylbenzene
  10. customcrystallized from 16 parts of methylbenzene

출처 및 근거

ORD 기록
ord-7a611e3a8b2a4244b930aae757826585
출처 데이터셋
uspto-grants-1979_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04175129

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