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

HRID 1704472
ノート
印刷プレビュー

反応式

HRID 1704472 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  1. stirringThe solution is further stirred
  2. temperaturerefluxed for 2 hours
  3. temperatureAfter cooling
  4. filtrationthe reaction mixture is 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

出典と根拠

ORDレコード
ord-34d19dc601ba4fbcaa8ab7925b42ef54
出典データセット
uspto-grants-1978_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04126687

反応ノート

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