Potassium Phosphate, Tribasic → HCID 69588726, 화합물

HRID 857019

반응식

HRID 857019 반응식
[C:1]([O:5][C:6](=[O:17])[NH:7][C@H:8]([C:10]1[CH:15]=[CH:14][CH:13]=[C:12](Br)[CH:11]=1)[CH3:9])([CH3:4])([CH3:3])[CH3:2].[CH3:18][N:19]([CH3:25])[C@@H:20]1[CH2:24][CH2:23][NH:22][CH2:21]1.[O-]P([O-])([O-])=O.[K+].[K+].[K+]>COCCOC.C(Cl)Cl.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[C:1]([O:5][C:6](=[O:17])[NH:7][CH:8]([C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([N:22]2[CH2:23][CH2:24][CH:20]([N:19]([CH3:25])[CH3:18])[CH2:21]2)[CH:11]=1)[CH3:9])([CH3:4])([CH3:3])[CH3:2]

참가 물질

7

반응물 3

HCID 62657Potassium Phosphate, TribasicHCID 2758521(3R)-(+)-3-(Dimethylamino)pyrrolidineHCID 56971804(S)-N-Boc-1-(3-bromophenyl)ethylamine

생성물 1

HCID 69588726HCID 69588726, 화합물수율 27%

시약·촉매·용매 3

HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 6344Dichloromethane용매HCID 80711,2-Dimethoxyethane용매

실험 절차

A mixture of (S )[1-(3-bromo-phenyl)-ethyl]-carbamic acid tert-butyl ester (6 g), (3R)-3-(dimethylamino)-pyrrolidine (4.56 g), Pd2(dba)3 (1.83 g), di-t-butyl-biphenylphosphine (600 mg), K3PO4 (8.48 g) in DME (40 mL) was stirred at reflux for 16 h. The reaction mixture was cooled down to room temperature, diluted with methylene chloride, and filtered. The filtrated was evaporated in vacuo, and the crude product was purified by Flash Chromatography using Biotage eluting with 20% MeOH in ethyl acetate to give the title compound (1.8 g) as an oil.

후처리

  1. temperatureat reflux for 16 h
  2. filtrationfiltered
  3. customThe filtrated was evaporated in vacuo
  4. customthe crude product was purified by Flash Chromatography
  5. washeluting with 20% MeOH in ethyl acetate

출처 및 근거

ORD 기록
ord-25c8f9ac53e244bba0ba6badd5929881
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07144881B2

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