HCID 178469787、化合物 → HCID 178524758、化合物
反応式
[CH2:1]([O:8][CH2:9][C:10]1[N:15]=[C:14]([OH:16])[C:13]([C:17]([O:19]CC)=[O:18])=[CH:12][N:11]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>[OH-].[K+]>[CH2:1]([O:8][CH2:9][C:10]1[N:15]=[C:14]([OH:16])[C:13]([C:17]([OH:19])=[O:18])=[CH:12][N:11]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
3
実験手順
A mixture of step C product (2-d) (10.0 g, crude) in a 3% KOH solution (200 mL) was stirred at 70° C. for 1 h, then cooled to room temperature. The material then washed with DCM (200 mL×2). The aqueous phase was acidified with 5% HCl to pH 1˜2, filtrated and then dried to afford product as a white solid (2-e) (6.2 g, 95% for 2 steps). 1H NMR (300 MHz, CD3OD): δ4.56 (s, 2H), 4.72 (s, 2H), 7.33-7.40 (m, 5H), 8.61 (s, 1H), LC-MS: (M+H)+ 261.
後処理
- washThe material then washed with DCM (200 mL×2)
- filtrationfiltrated
- customdried
出典と根拠
- ORDレコード
- ord-55a028c6aac046718b95400de4cbfb11
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09034851B2
反応ノート
読み込み中…