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

Sodium Carbonate → HCID 59765138, 화합물

HRID 536206
노트
인쇄 미리보기

반응식

HRID 536206 반응식
[Cl:1][C:2]1[C:7](I)=[C:6]([NH2:9])[CH:5]=[CH:4][N:3]=1.[Cl-].[Li+].C(=O)([O-])[O-].[Na+].[Na+].[CH3:18][O:19][C:20]1[CH:21]=[C:22]([C:26]#[C:27][Si:28]([CH3:31])([CH3:30])[CH3:29])[CH:23]=[CH:24][CH:25]=1>CN(C=O)C.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].O>[Cl:1][C:2]1[C:7]2[C:26]([C:22]3[CH:23]=[CH:24][CH:25]=[C:20]([O:19][CH3:18])[CH:21]=3)=[C:27]([Si:28]([CH3:31])([CH3:29])[CH3:30])[NH:9][C:6]=2[CH:5]=[CH:4][N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 10340Sodium CarbonateHCID 433294Lithium ChlorideHCID 4407093(3-Methoxyphenylethynyl)trimethylsilaneHCID 242292082-Chloro-3-iodopyridin-4-amine

생성물 1

HCID 59765138HCID 59765138, 화합물

시약·촉매·용매 3

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
촉매
HCID 962Water용매
HCID 6228Dimethylformamide용매

실험 절차

7.6 g (30 mmol) of 2-chloro-3-iodopyridin-4-ylamine from Example B1, 1.7 g (41 mmol) of lithium chloride and 15.9 g (120 mmol) of sodium carbonate are dissolved in 100 ml of DMF, and 8 g (39 mmol) of commercial (3-methoxyphenyl)ethynyltrimethylsilane and 4.9 g (6 mmol) of commercial Pd(dppf)2Cl2*H2Cl2 are added at 100° C. under nitrogen. The mixture is stirred at the temperature indicated for 12 h and subsequently poured at room temperature (RT) into water and extracted with ethyl acetate. The organic phase is concentrated and purified by chromatography over silica gel. The combined product fractions (5.3 g; 53%; pale-brown oil) are used for the subsequent reaction.

후처리

  1. extractionextracted with ethyl acetate
  2. concentrationThe organic phase is concentrated
  3. custompurified by chromatography over silica gel
  4. customThe combined product fractions (5.3 g; 53%; pale-brown oil) are used for the subsequent reaction

출처 및 근거

ORD 기록
ord-7d482365f65d4cef9d1d7cbe1af86923
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08859581B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트