反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8][C@H:9]([C:15]1[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=1)[C@H:10]([OH:14])[C:11]([O-:13])=[O:12].C[C@H]([NH3+])C1C=CC=CC=1.Cl>O>[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8][C@H:9]([C:15]1[CH:16]=[CH:17][C:18]([O:21][CH3:22])=[CH:19][CH:20]=1)[C@H:10]([OH:14])[C:11]([OH:13])=[O:12]参加物
4
実験手順
Dissolve the (-)-salt 4 (42.85 g, 97.26 mmol) in boiling water (430 mL). Add hot 1N HCl (98 mL). Reflux for 1 min. Cool the mixture in an ice-water bath and stir vigourously to precipitate. Check (and adjust if necessary) the pH of the solution to 5.0 (pH meter). Collect the solid by filtration. Wash with water and dry in vacuo at 40° C. to obtain the title compound 5 (24.85 g, 80%). m.p. 175°-176° C. [α]D23 -362.8° (1.2 DMF).
後処理
- temperatureReflux for 1 min
- temperatureCool the mixture in an ice-water bath
- customto precipitate
- customCollect the solid
- filtrationby filtration
- washWash with water
- customdry in vacuo at 40° C.
出典と根拠
- ORDレコード
- ord-91f5817949094ac49a86750469c7a62c
- 出典データセット
- uspto-grants-1996_12
- 特許番号
- US05580867
関連ノート
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