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

3-Chloro-5-[(5-chloro-3,6-difluoropyridin-2-yl)oxy]benzonitrile → HCID 178509961, 화합물

HRID 1952337
노트
인쇄 미리보기

반응식

HRID 1952337 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([O:10][C:11]2[C:16]([F:17])=[CH:15][C:14]([Cl:18])=[C:13](F)[N:12]=2)[CH:9]=1)[C:5]#[N:6].[NH2:20][CH2:21][C:22]1[C:30]2[C:25](=[N:26][CH:27]=[CH:28][CH:29]=2)[NH:24][N:23]=1>CN1C(=O)CCC1.O>[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([O:10][C:11]2[C:16]([F:17])=[CH:15][C:14]([Cl:18])=[C:13]([NH:20][CH2:21][C:22]3[C:30]4[C:25](=[N:26][CH:27]=[CH:28][CH:29]=4)[NH:24][N:23]=3)[N:12]=2)[CH:9]=1)[C:5]#[N:6]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 595297603-Chloro-5-[(5-chloro-3,6-difluoropyridin-2-yl)oxy]benzonitrileHCID 178510691HCID 178510691, 화합물

생성물 1

HCID 178509961HCID 178509961, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
90 °C

실험 절차

A solution of 50 mg (0.166 mmol) of 1-6 and 25 mg (0.166 mmol) of 1-3 in 1.5 mL of dry NMP was heated with stirring at 90° C. under nitrogen. After 7 hours, the reaction was stopped and cooled. The reaction mixture was diluted with water, and extracted twice with EtOAc. The combined EtOAc extracts were washed with water and brine, dried, filtered, and concentrated in vacuo to give a crude oil. The crude product was purified by reversed phase preparative HPLC on a Gilson apparatus to give the title product as a white amorphous solid. MS M+1=430. 1H NMR (CDCl3): 4.77 (d, 2H), 5.60 (br m, 1H), 7.17 (q, 1H), 7.34 (m, 1H), 7.36 (m, 1H), 7.39 (m, 1H), 7.50 (d, 1H), 8.01 (dd, 1H), 8.53 (m, 1H), 10.5-11.5 (br, 1H).

후처리

  1. temperaturecooled
  2. extractionextracted twice with EtOAc
  3. washThe combined EtOAc extracts were washed with water and brine
  4. customdried
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customto give a crude oil
  8. customThe crude product was purified by reversed phase preparative HPLC on a Gilson apparatus

출처 및 근거

ORD 기록
ord-247f4a4a37dd41c881a7cdfe06cfa521
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08404856B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트