Hydrogen Bromide → HCID 69735974、化合物
反応式
C[O:2][C:3]([C:5]1[C:16]2[C:15]3[N:11]([CH:12]=[CH:13][N:14]=3)[CH2:10][CH2:9][C:8]=2[NH:7][CH:6]=1)=[O:4].[BrH:17]>>[BrH:17].[N:14]1[CH:13]=[CH:12][N:11]2[C:15]=1[C:16]1[C:5]([C:3]([OH:4])=[O:2])=[CH:6][NH:7][C:8]=1[CH2:9][CH2:10]2参加物
3
実験手順
A solution of 5,6-dihydro-4H-1,3a,6-triaza-as-indacene-8-carboxylic acid methyl ester (516 mg) and 48% hydrobromic acid (5 mL) is heated at 60° for 60 hours. The mixture is cooled to room temperature and concentrated in vacuo. The residue is slurried with diethyl ether and the ether is decanted off. This is repeated until no more color is visible in the ether layer. The remaining solid is dried in vacuo to give 5,6-dihydro-4H-1,3a,6-triaza-as-indacene-8-carboxylic acid hydrobromide, 350 mg, brown solid: 1H NMR(DMSO-d6) 3.17 (2H, t), 4.40 (2H, t), 7.35 (1H, d), 7.57 (1H, d), 7.63 (1H, s), 12.34 (1H, s), 12.45 (1H, s).
後処理
- concentrationconcentrated in vacuo
- customthe ether is decanted off
- customThe remaining solid is dried in vacuo
出典と根拠
- ORDレコード
- ord-6f7025ef8b134be0b03286e5ce9b585e
- 出典データセット
- uspto-grants-2005_09
- 特許番号
- US06949562B2
反応ノート
読み込み中…