Potassium Phosphate, Tribasic → HCID 69588726、化合物

HRID 857019

反応式

HRID 857019 の反応式
[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]

参加物

7

反応物 3

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

生成物 1

HCID 69588726HCID 69588726、化合物収率 27%

試薬・触媒・溶媒 3

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 6344Dichloromethane溶媒HCID 80711,2-Dimethoxyethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-25c8f9ac53e244bba0ba6badd5929881
出典データセット
uspto-grants-2006_12
特許番号
US07144881B2

関連ノート

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