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

Sodium Hydroxide → N'-[6-(4-chloro-3-trifluoromethyl-phenoxy)-2-methyl-5-trimethylsilanylethynyl-pyridin-3-yl]-N-ethyl-N-methyl-formamidine

HRID 1894640
노트
인쇄 미리보기

반응식

HRID 1894640 반응식
[CH2:1]([N:3]([CH3:6])[CH:4]=O)[CH3:2].[Cl-].[P+]=O.[Cl:10][C:11]1[CH:31]=[CH:30][C:14]([O:15][C:16]2[N:21]=[C:20]([CH3:22])[C:19]([NH2:23])=[CH:18][C:17]=2[C:24]#[C:25][Si:26]([CH3:29])([CH3:28])[CH3:27])=[CH:13][C:12]=1[C:32]([F:35])([F:34])[F:33].[OH-].[Na+]>ClCCl>[Cl:10][C:11]1[CH:31]=[CH:30][C:14]([O:15][C:16]2[N:21]=[C:20]([CH3:22])[C:19]([N:23]=[CH:4][N:3]([CH2:1][CH3:2])[CH3:6])=[CH:18][C:17]=2[C:24]#[C:25][Si:26]([CH3:29])([CH3:27])[CH3:28])=[CH:13][C:12]=1[C:32]([F:34])([F:33])[F:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 350667N-ethyl-N-methylformamideHCID 581534926-(4-Chloro-3-trifluoromethyl-phenoxy)-2-methyl-5-trimethylsilanylethynyl-pyridin-3-ylamineHCID 178527006HCID 178527006, 화합물

생성물 1

HCID 25159299N'-[6-(4-chloro-3-trifluoromethyl-phenoxy)-2-methyl-5-trimethylsilanylethynyl-pyridin-3-yl]-N-ethyl-N-methyl-formamidine

시약·촉매·용매

1
HCID 6344Dichloromethane용매2회

실험 절차

In a 10 ml single-necked round-bottomed flask, 3.1 mg. of ethylmethylformamide is solubilized in 0.25 ml of dry dichloromethane at ambient temperature (colourless solution). Under stirring, 0.0032 ml of phosphorous oxide chloride is added dropwise by syringe. Stirring at ambient temperature is continued for 1.0 hour, whereupon a pink-orange solution is obtained. To this solution, 7.0 mg of 6-(4-chloro-3-trifluoromethyl-phenoxy)-2-methyl-5-trimethylsilanylethynyl-pyridin-3-ylamine dissolved in 0.75 ml of dry dichloromethane is added dropwise by syringe, giving a yellow solution. Stirring is continued at room temperature for 2.5 hours. The mixture is then poured into ice/water (pH=2, water phase). 2 M aqueous NaOH is then added to get a pH of about 11 and stirring is continued for 15 minutes. The mixture is then extracted with two 10 ml portions of diethyl ether. The combined organic phases are then dried over sodium sulfate, filtered and the solvent is removed in vacuo to obtain 6.0 mg of the compound as a yellow oil. RP HPLC: retention time of compound: 1.61 minutes.

후처리

  1. stirringStirring at ambient temperature
  2. customis obtained
  3. additionis added dropwise by syringe
  4. customgiving a yellow solution
  5. stirringStirring
  6. waitis continued at room temperature for 2.5 hours
  7. customto get a pH of about 11
  8. stirringstirring
  9. waitis continued for 15 minutes
  10. extractionThe mixture is then extracted with two 10 ml portions of diethyl ether
  11. dry with materialThe combined organic phases are then dried over sodium sulfate
  12. filtrationfiltered
  13. customthe solvent is removed in vacuo

출처 및 근거

ORD 기록
ord-9f264b347a48407fba57eed7b65c35a0
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08513286B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트