Acetic Acid → N-[(5-bromo-1,3-thiazol-2-yl)carbamoyl]-4-[(3,4-dichloro-1-methyl-1H-pyrazol-5-yl)oxy]benzenesulfonamide

HRID 252242

반응식

HRID 252242 반응식
[Cl:1][C:2]1[C:6]([Cl:7])=[N:5][N:4]([CH3:8])[C:3]=1[O:9][C:10]1[CH:15]=[CH:14][C:13]([S:16]([NH2:19])(=[O:18])=[O:17])=[CH:12][CH:11]=1.[Br:20][C:21]1[S:25][C:24]([N:26](C(OC2C=CC=CC=2)=O)[C:27](OC2C=CC=CC=2)=[O:28])=[N:23][CH:22]=1.C1CCN2C(=NCCC2)CC1.C(O)(=O)C>CN(C=O)C.O>[Br:20][C:21]1[S:25][C:24]([NH:26][C:27]([NH:19][S:16]([C:13]2[CH:12]=[CH:11][C:10]([O:9][C:3]3[N:4]([CH3:8])[N:5]=[C:6]([Cl:7])[C:2]=3[Cl:1])=[CH:15][CH:14]=2)(=[O:18])=[O:17])=[O:28])=[N:23][CH:22]=1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 14782454-(4,5-Dichloro-2-methylpyrazol-3-yl)oxybenzenesulfonamideHCID 66858288Diphenyl (5-bromo-1,3-thiazol-2-yl)imidodicarbonate

생성물 1

HCID 24780160N-[(5-bromo-1,3-thiazol-2-yl)carbamoyl]-4-[(3,4-dichloro-1-methyl-1H-pyrazol-5-yl)oxy]benzenesulfonamide

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매2회

실험 절차

4-(4,5-dichloro-2-methyl-2H-pyrazol-3-yloxy)-benzenesulfonamide (77.3 mg, 0.24 mmol) and diphenyl (5-bromo-1,3-thiazol-2-yl)imidodicarbonate (100 mg, 0.24 mmol) were suspended in DMF (0.4 ml). A solution of DBU (0.04 ml, 0.26 mmol) in DMF (0.1 ml) was added dropwise and the clear mixture was shaken for 1.5 h at rt and kept overnight at 4° C. The mixture was acidified using acetic acid (0.2 ml) and diluted with water (0.2 ml) and purified directly using preparative RP(C18)chromatography: lyophilisate 9 mg, MS: m/e 523.8 (MH−).

후처리

  1. waitkept overnight at 4° C
  2. custompurified directly

출처 및 근거

ORD 기록
ord-b834cd58a75a4f18997d8625d3fa8c17
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07868030B2

연결된 노트

불러오는 중…