Hydrochloric Acid → N-[2-(Hydroxy-2-oxo-3H-1,3-benzothiazol-7-yl)ethyl]-3-[2-(2-phenylethoxy)ethylaminosulphonyl]propanamide
反応式
[C:1]1([CH2:7][CH2:8][O:9][CH2:10][CH2:11][NH:12][S:13]([CH2:16][CH2:17][C:18]([OH:20])=O)(=[O:15])=[O:14])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.O[C:23]1[C:28]2[NH:29][C:30](=[O:32])[S:31][C:27]=2[CH:26]=[CH:25][CH:24]=1.F[P-](F)(F)(F)(F)F.Br[P+](N1CCCC1)(N1CCCC1)[N:42]1CC[CH2:44][CH2:43]1.C(N(C(C)C)CC)(C)C.Cl.CN(C)C=[O:70]>>[OH:70][N:29]1[C:28]2[CH:23]=[CH:24][CH:25]=[C:26]([CH2:44][CH2:43][NH:42][C:18](=[O:20])[CH2:17][CH2:16][S:13]([NH:12][CH2:11][CH2:10][O:9][CH2:8][CH2:7][C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)(=[O:14])=[O:15])[C:27]=2[S:31][C:30]1=[O:32]参加物
7
反応物 6
生成物 1
反応条件
- 温度
- -15 °C
実験手順
A solution of the product from step b) (3.89 g), 7-2-aminoethyl)4-hydroxy-1,3-benzothiazol-2(3H)-one hydrochloride (3.22 g), bromotripyrrolidinophosphonium hexafluorophosphate, PyBroP, (6.32 g) in dimethylformamide (50 ml) was cooled to -15° C. and diisopropylethylamine (9.0 ml) was added dropwise over 5 minutes. The solution was stirred at -15° C. for 5 min then allowed to warm to 13° C. over 4 hours. This mixture was then added dropwise over 40 min to dilute hydrochloric acid (2N, 500 ml) and after stirring over the weekend the solid was collected by filtration. This solid was dried in vacuo to give the subtitle compound (4.5 g).
後処理
- temperatureto warm to 13° C. over 4 hours
- stirringafter stirring over the weekend the solid
- filtrationwas collected by filtration
- customThis solid was dried in vacuo
出典と根拠
- ORDレコード
- ord-adfb7b5e8e17413a913a00b7880a3751
- 出典データセット
- uspto-grants-1999_10
- 特許番号
- US05973167
反応ノート
読み込み中…