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Methanesulfonic Acid → HCID 67458340, 화합물

HRID 554819
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HRID 554819 반응식
C(O[C:6]([NH:8][CH2:9][C@H:10]([CH2:14][C:15]1[CH:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:16]=1[O:22][CH3:23])[C:11]([OH:13])=[O:12])=O)(C)(C)C.CS(O)(=O)=O.[CH3:29][O:30][C:31]1[CH:38]=[C:37]([O:39][CH3:40])[CH:36]=[C:35]([O:41][CH3:42])[C:32]=1C=O.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[OH-].[Na+]>C(OCC)(=O)C.C(N(CC)CC)C>[Cl:21][C:19]1[CH:18]=[CH:17][C:16]([O:22][CH3:23])=[C:15]([CH:20]=1)[CH2:14][C@@H:10]([CH2:9][NH:8][CH2:6][C:32]1[C:35]([O:41][CH3:42])=[CH:36][C:37]([O:39][CH3:40])=[CH:38][C:31]=1[O:30][CH3:29])[C:11]([OH:13])=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 6395Methanesulfonic AcidHCID 14798Sodium HydroxideHCID 700192,4,6-TrimethoxybenzaldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 66935162(2S)-3-[(tert-butoxycarbonyl)amino]-2-(5-chloro-2-methoxybenzyl)propanoic acid

생성물 1

HCID 67458340HCID 67458340, 화합물

시약·촉매·용매 2

HCID 8471Triethylamine용매HCID 8857Ethyl Acetate용매

실험 절차

(2S)-3-[(tert-butoxycarbonyl)amino]-2-(5-chloro-2-methoxybenzyl)propionic acid (10g) was dissolved in ethyl acetate (120 ml), then methane sulfonic acid (9.4 ml) was added at room temperature, and the resulting mixture was stirred at that temperature for 2 hours. To the reaction solution was added triethylamine (20.3 ml), and the mixture was stirred for 13 hours. Then 2,4,6-trimethoxybenzaldehyde (5.7 g) was added and the mixture was stirred for 30 minutes. Next, to the reaction solution, sodium triacetoxyborohydride (9.3 g) was added and the mixture was stirred for 2 hours. To the reaction solution, a 1N aqueous sodium hydroxide solution was added, and the layers were separated. The aqueous layer was extracted again with ethyl acetate. The organic layer was washed with a 1N aqueous sodium hydroxide solution, then the appeared precipitated crystals were collected by filtration and dried to obtain the title compound (11.5 g) as a colorless crystal.

후처리

  1. stirringthe mixture was stirred for 13 hours
  2. stirringthe mixture was stirred for 30 minutes
  3. stirringthe mixture was stirred for 2 hours
  4. customthe layers were separated
  5. extractionThe aqueous layer was extracted again with ethyl acetate
  6. washThe organic layer was washed with a 1N aqueous sodium hydroxide solution
  7. customthe appeared precipitated crystals
  8. filtrationwere collected by filtration
  9. customdried

출처 및 근거

ORD 기록
ord-a936a41559074d77bac253747f5ebdbc
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08049006B2

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