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Methanesulfonyl chloride → 1,3-dihydro-1-(3-hydroxypropyl)-2H-benzimidazol-2-one methanesulfonate

HRID 1704471
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HRID 1704471 반응식
[OH2:1].[OH:2][CH2:3][CH2:4][CH2:5][N:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[NH:8][C:7]1=[O:15].[CH3:16][S:17](Cl)(=[O:19])=[O:18]>N1C=CC=CC=1>[CH3:16][S:17]([OH:19])(=[O:1])=[O:18].[OH:2][CH2:3][CH2:4][CH2:5][N:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[NH:8][C:7]1=[O:15]
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참가 물질

4

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 203855841,3-dihydro-1-(3-hydroxypropyl)-2H-benzimidazol-2-one hydrate

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To a solution of 52.5 parts of 1,3-dihydro-1-(3-hydroxypropyl)-2H-benzimidazol-2-one hydrate in 200 parts of pyridine is added dropwise 63 parts of methanesulfonyl chloride. The mixture is stirred and cooled on the air for 2 hours. The pyridine is evaporated. To the residue is added 500 parts of water and the formed precipitate is filtered off. It is dissolved in 350 parts of trichloromethane. This solution is dried over magnesium sulfate and evaporated. The residue is crystallized from 40 parts of methylbenzene, yielding 25.5 parts of 1,3-dihydro-1-(3-hydroxypropyl)-2H-benzimidazol-2-one methanesulfonate; mp. 118°-120° C.

후처리

  1. temperaturecooled on the air for 2 hours
  2. customThe pyridine is evaporated
  3. additionTo the residue is added 500 parts of water
  4. filtrationthe formed precipitate is filtered off
  5. dissolutionIt is dissolved in 350 parts of trichloromethane
  6. dry with materialThis solution is dried over magnesium sulfate
  7. customevaporated
  8. customThe residue is crystallized from 40 parts of methylbenzene

출처 및 근거

ORD 기록
ord-1289ec11f6af4ee5a9d10d8f880800c7
출처 데이터셋
uspto-grants-1978_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04126687

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