홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Potassium Phosphate, Tribasic → 5-(3-Bromo-1,2,4-thiadiazol-5-yl)-3-chloro-2-[(1-methylethyl)oxy]pyridine

HRID 1942676
노트
인쇄 미리보기

반응식

HRID 1942676 반응식
[Cl:1][C:2]1[C:3]([O:17][CH:18]([CH3:20])[CH3:19])=[N:4][CH:5]=[C:6](B2OC(C)(C)C(C)(C)O2)[CH:7]=1.[Br:21][C:22]1[N:26]=[C:25](Cl)[S:24][N:23]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].C(Cl)Cl>[Br:21][C:22]1[N:26]=[C:25]([C:6]2[CH:7]=[C:2]([Cl:1])[C:3]([O:17][CH:18]([CH3:19])[CH3:20])=[N:4][CH:5]=2)[S:24][N:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 62657Potassium Phosphate, TribasicHCID 27250533-Bromo-5-chloro-1,2,4-thiadiazoleHCID 580424553-Chloro-2-isopropoxy-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-YL)pyridine

생성물 1

HCID 584941105-(3-Bromo-1,2,4-thiadiazol-5-yl)-3-chloro-2-[(1-methylethyl)oxy]pyridine수율 96.4%

시약·촉매·용매 1

HCID 178418807
HCID 178418807, 화합물
촉매

실험 절차

3-chloro-2-[(1-methylethyl)oxy]-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine (D108) (1.2 g, 4.03 mmol), 3-bromo-5-chloro-1,2,4-thiadiazole (1.609 g, 8.06 mmol), tripotassium phosphate (2.57 g, 12.10 mmol) and PdCl2(dppf)-CH2Cl2 adduct (0.329 g, 0.403 mmol) were heated by Biotage Initiator to 80° C. for 1 hr. The reaction mixture was concentrated and the slurry was diluted with ethyl acetate. The resulted solution was washed with water, dried and purified by ISCO column chromatography to afford 5-(3-bromo-1,2,4-thiadiazol-5-yl)-3-chloro-2-[(1-methylethyl)oxy]pyridine (D109) (1.3 g). δH (CDCl3, 400 MHz): 1.43 (6H, d), 5.45 (1H, m), 8.21 (1H, d), 8.59 (1H, d). MS (ES): C10H9BrClN3OS requires 332.9. found 334.0 (M+H+).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. additionthe slurry was diluted with ethyl acetate
  3. washThe resulted solution was washed with water
  4. customdried
  5. custompurified by ISCO column chromatography

출처 및 근거

ORD 기록
ord-4f6fd25b7bdc45ea8f0951d865c11940
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08389508B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트