Hydrochloric Acid → Diethyl(2-sulfamoyl-6-benzothiazolyl)phosphate

HRID 1263215ノート

反応式

HRID 1263215 の反応式
[OH:1][C:2]1[CH:14]=[CH:13][C:5]2[N:6]=[C:7]([S:9]([NH2:12])(=[O:11])=[O:10])[S:8][C:4]=2[CH:3]=1.[CH3:15][CH2:16][O:17][P:18](Cl)([O:20][CH2:21][CH3:22])=[O:19].Cl>CN(C)C1C=CN=CC=1.N1C=CC=CC=1>[CH3:15][CH2:16][O:17][P:18]([O:1][C:2]1[CH:14]=[CH:13][C:5]2[N:6]=[C:7]([S:9]([NH2:12])(=[O:11])=[O:10])[S:8][C:4]=2[CH:3]=1)([O:20][CH2:21][CH3:22])=[O:19]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 13139Diethyl chlorophosphate2 回HCID 68521296-Hydroxy-1,3-benzothiazole-2-sulfonamide

生成物 1

HCID 13343650Diethyl(2-sulfamoyl-6-benzothiazolyl)phosphate収率 31.4%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 1049Pyridine溶媒

反応条件

温度
25 °C

実験手順

To a stirred solution of 6-hydroxy-2-benzothiazolesulfonamide (2.3 g, 0.01 mole) and 4-dimethylaminopyridine (200 mg) in pyridine (20 ml) was added chlorodiethylphosphate (1.45 ml, 0.01 mole). After stirring for 4 hours at 25° C. additional chlorodiethylphosphate (1.5 ml) was added and the reaction mixture was stirred at 25° C. for 18 hours then poured into ice water and excess hydrochloric acid to give 1.15 g of diethyl(2-sulfamoyl-6-benzothiazolyl)phosphate m.p. 142°-144° C. after recrystallization from ethylene chloride.

後処理

  1. additionwas added

出典と根拠

ORDレコード
ord-cd78816f0fae4ad7b32e21a0e00b579c
出典データセット
uspto-grants-1984_06
特許番号
US04456599

反応ノート

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