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Hydrochloric Acid → 5-[3-(3-Hydroxyphenyl)indolin-1-ylcarbonyl]-4,5,6,7-tetrahydrobenzimidazole

HRID 1585221
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HRID 1585221 반응식
Cl.[N:2]1[C:6]2[CH2:7][CH2:8][CH:9]([C:11]([OH:13])=O)[CH2:10][C:5]=2[NH:4][CH:3]=1.S(Cl)(Cl)=O.[OH:18][C:19]1[CH:20]=[C:21]([CH:25]2[C:33]3[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=3)[NH:27][CH2:26]2)[CH:22]=[CH:23][CH:24]=1.C(=O)(O)[O-].[Na+]>O1CCCC1.CN(C)C=O>[OH:18][C:19]1[CH:20]=[C:21]([CH:25]2[C:33]3[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=3)[N:27]([C:11]([CH:9]3[CH2:8][CH2:7][C:6]4[N:2]=[CH:3][NH:4][C:5]=4[CH2:10]3)=[O:13])[CH2:26]2)[CH:22]=[CH:23][CH:24]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 24386Thionyl ChlorideHCID 516892Sodium BicarbonateHCID 110301834,5,6,7-Tetrahydro-1H-benzoimidazole-5-carboxylic acidHCID 212222863-(3-Hydroxyphenyl)indoline

생성물 1

HCID 99287795-[3-(3-Hydroxyphenyl)indolin-1-ylcarbonyl]-4,5,6,7-tetrahydrobenzimidazole
수율 56.8%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 1.99 g of hydrochloride (racemic form) of 4,5,6,7-tetrahydrobenzimidazole-5-carboxylic acid, 0.15 ml of dimethyl formamide and 20 ml of thionyl chloride was refluxed for three hours. The resultant reaction solution was distilled to dryness under a reduced pressure. The residue consequently formed was added to a solution of 2.07 g of (+)-3-(3-hydroxyphenyl)indoline in 75 ml of tetrahydrofuran. This reaction solution was stirred at room temperature for 12 hours, then weakly alkalinized by addition of the saturated aqueous sodium bicarbonate solution, and extracted with chloroform. The chloroform layer was dried over anhydrous magnesium sulfate and then distilled. The residue was refined by silica gel column chromatography to obtain 2.00 g of 5-[{3-(3-hydroxyphenyl)indolin-1-ylcarbonyl}]-4,5,6,7-tetrahydrobenzimidazole (56.8%) as an epimer mixture.

후처리

  1. temperaturewas refluxed for three hours
  2. customThe resultant reaction solution
  3. distillationwas distilled to dryness under a reduced pressure
  4. customThe residue consequently formed
  5. extractionextracted with chloroform
  6. dry with materialThe chloroform layer was dried over anhydrous magnesium sulfate
  7. distillationdistilled

출처 및 근거

ORD 기록
ord-e4b70f7f761c4e15a786b0f60277fef0
출처 데이터셋
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05936098

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