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

Potassium Carbonate → ethyl 6-chloro-7-[(3,3-dimethylbutyl)amino]-2-(trifluoromethyl)-2H-chromene-3-carboxylate

HRID 855077
노트
인쇄 미리보기

반응식

HRID 855077 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1F)[O:8][CH:7]([C:13]([F:16])([F:15])[F:14])[C:6]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:5]2.[CH3:22][C:23]([CH3:28])([CH3:27])[CH2:24][CH2:25][NH2:26].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[NH:26][CH2:25][CH2:24][C:23]([CH3:28])([CH3:27])[CH3:22])[O:8][CH:7]([C:13]([F:16])([F:15])[F:14])[C:6]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:5]2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 197093,3-DimethylbutylamineHCID 21883602ethyl 6-chloro-7-fluoro-2-(trifluoromethyl)-2H-chromene-3-carboxylate

생성물 1

HCID 69518833ethyl 6-chloro-7-[(3,3-dimethylbutyl)amino]-2-(trifluoromethyl)-2H-chromene-3-carboxylate수율 87%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
90 °C

실험 절차

A mixture of ethyl 6-chloro-7-fluoro-2-(trifluoromethyl)-2H-chromene-3-carboxylate (Example 7a, Step 2) (0.5 g, 1.54 mmole) and 3,3-dimethylbutylamine (0.21 mL, 1.54 mmole) was dissolved in anhydrous DMF (5 mL), warmed to 90° C. and treated with K2CO3 (0.25 g, 1.84 mmole). The mixture was maintained at 90° C. for 24 hrs, cooled to room temperature, filtered through celite and condensed to a viscous oil. The oil was purified by flash chromatography (silica gel) with 40% methylene chloride in hexane to give light yellow solid (0.54 g, 87%): GCMS ml/z 405.00 (M+). 1H NMR (CDCl3/400 MHz) 7.58 (s, 1H), 7.08 (s, 1H), 6.22 (s, 1H), 5.64 (q, 1H, J=7.0 Hz), 4.26 (m, 2H), 3.16 (m, 2H), 1.57 (m, 2H), 1.33 (m, 3H), 0.98 (s, 9H).

후처리

  1. temperatureThe mixture was maintained at 90° C. for 24 hrs
  2. temperaturecooled to room temperature
  3. filtrationfiltered through celite and condensed to a viscous oil
  4. customThe oil was purified by flash chromatography (silica gel) with 40% methylene chloride in hexane

출처 및 근거

ORD 기록
ord-ba0417181d9145fe87a697014a5f22c4
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07259266B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트