反応式
[C:1]([NH:5][C:6]([C:8]1[CH:13]=[N:12][CH:11]=[CH:10][N:9]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[Cl-]>CO>[C:1]([NH:5][C:6]([C@@H:8]1[CH2:13][NH:12][CH2:11][CH2:10][NH:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]参加物
実験手順
0.5 g (2.7 mmol) of pyrazinecarboxylic acid tert-butylamide (prepared according to Example 3), 26.9 mg (58 μmol) of bicyclo[2.2.1]hepta-2,5-dienerhodium(I) chloride dimer and 72 mg (121 μmol) of 1-[1 (R)-(dicyclohexylphosphino)ethyl]-2(S)-(diphenylphosphino)ferrocene were placed in an autoclave under argon. After the addition of 10 ml of degassed methanol, the autoclave was flushed three times with argon and twice with hydrogen. A hydrogen pressure of 50 bar was then applied. Hydrogenation was carried out at 70° C. for 20 hours. The autoclave was depressurized and flushed with nitrogen. The solvent was completely distilled off. The yield of the title compound was 0.50 g. A conversion of 80 percent was determined by NMR. The enantiomeric excess (ee) was 77.6 percent according to GC analysis.
後処理
- customthe autoclave was flushed three times with argon
- customflushed with nitrogen
- distillationThe solvent was completely distilled off
出典と根拠
- ORDレコード
- ord-5c436cb535344985a936f615956edea5
- 出典データセット
- uspto-grants-1999_08
- 特許番号
- US05945534
関連ノート
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