Methyl iodide → HCID 58748311、化合物
反応式
[C:1]([O:5][C:6]([N:8]1[CH2:12][C@@H:11]([OH:13])[C@H:10]([C:14]#[N:15])[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH3:16]I>C1COCC1>[C:1]([O:5][C:6]([N:8]1[CH2:12][C@@H:11]([O:13][CH3:16])[C@H:10]([C:14]#[N:15])[CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]参加物
4
反応条件
- 温度
- 50 °C
実験手順
80.2 A suspension of (3S,4S)-3-cyano-4-hydroxy-pyrrolidine-1-carboxylic acid tert-butyl ester (212 mg) in 10 ml of THF and 2.32 g of Ag2O and 0.62 ml of CH3I was heated in a sealed tube to 50° C. for 16 h. The suspension was filtered and the filtrate chromatographed on silica (heptane/AcOEt, 3:1) to give 161 mg of (3S,4S)-3-cyano-4-methoxy-pyrrolidine-1-carboxylic acid tert-butyl ester. Colorless oil. MS 171.4 ([M-isobutene+H]+)
後処理
- filtrationThe suspension was filtered
- customthe filtrate chromatographed on silica (heptane/AcOEt, 3:1)
出典と根拠
- ORDレコード
- ord-6f44fea281454aa29945c2c4c316cd01
- 出典データセット
- uspto-grants-2010_10
- 特許番号
- US07820699B2
反応ノート
読み込み中…