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Hydrochloric Acid → 3-Hydroxy-2-(4-methoxyphenyl)-2,3-dihydro-1,5-benzothiazepin-4(5H)-one, (2S,3S)-

HRID 1457253
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HRID 1457253 반응식
COC1C=CC([C@@H]2O[C@H]2C(N)=O)=CC=1.NC1C=CC=CC=1S.N[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[S:30][CH:31]([C:37]1[CH:42]=[CH:41][C:40]([O:43][CH3:44])=[CH:39][CH:38]=1)[CH:32]([OH:36])[C:33]([NH2:35])=[O:34].Cl>CO.ClC1C=CC=CC=1>[OH:36][C@H:32]1[C:33](=[O:34])[NH:35][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=2[S:30][C@H:31]1[C:37]1[CH:42]=[CH:41][C:40]([O:43][CH3:44])=[CH:39][CH:38]=1
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참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 87132-AminothiophenolHCID 10821599(2R,3S)-3-(4-methoxyphenyl)-2,3-epoxypropionamideHCID 538426453-(2-Aminophenylthio)-2-hydroxy-3-(4-methoxyphenyl)propionamide

생성물 1

HCID 27336733-Hydroxy-2-(4-methoxyphenyl)-2,3-dihydro-1,5-benzothiazepin-4(5H)-one, (2S,3S)-수율 19.6%

시약·촉매·용매 2

HCID 887Methanol용매
HCID 7964Chlorobenzene용매

실험 절차

A mixture of (2R,3S)-3-(4-methoxyphenyl)-2,3-epoxypropionamide (15.46 g) and chlorobenzene (309 ml) is refluxed with heating under nitrogen atmosphere. When the reflux is started, a solution of 2-aminothiophenol (11.02 g) and ferric chloride hexahydrate (2.16 mg) in methanol (0.1 ml) is added immediately to the reaction mixture, and the mixture is stirred at the same temperature for 5 minutes to give a reaction mixture containing 3-(2-aminophenylthio)-2-hydroxy-3-(4-methoxyphenyl)propionamide (24.24 g) [(2S,3S)/(2S,3R)=91.3/8.7]. A quarter of the mixture is obtained, and 35% hydrochloric acid (1.04 g) is added thereto. The mixture is refluxed for 13 hours to remove the solvent. The remaining chlorobenzene is evaporated from the mixture, and methanol (25 ml) is added to the residue. The mixture is refluxed for one hour, allowed to cool to room temperature, and further cooled at 3° C. overnight. The precipitated crystals are collected by filtration, washed with chilled methanol, and dried at 50° C. to give (2S,3S)-2,3-dihydro-3-hydroxy-2-(4-methoxyphenyl)-1,5-benzothiazepin-4(5H)-one (4.49 g).

후처리

  1. temperatureis refluxed
  2. temperaturewith heating under nitrogen atmosphere
  3. customto give a reaction mixture
  4. customA quarter of the mixture is obtained
  5. temperatureThe mixture is refluxed for 13 hours
  6. customto remove the solvent
  7. customThe remaining chlorobenzene is evaporated from the mixture, and methanol (25 ml)
  8. additionis added to the residue
  9. temperatureThe mixture is refluxed for one hour
  10. temperaturefurther cooled at 3° C. overnight
  11. filtrationThe precipitated crystals are collected by filtration
  12. washwashed with chilled methanol
  13. customdried at 50° C.

출처 및 근거

ORD 기록
ord-b74fd088aa3f4f84ab3845dcb76904ab
출처 데이터셋
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05847122

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