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

Diethylamine → HCID 86612229, 화합물

HRID 30015
노트
인쇄 미리보기

반응식

HRID 30015 반응식
C(=O)([O-])[O-].[K+].[K+].[CH2:7]([NH:9][CH2:10][CH3:11])[CH3:8].[Cl:12][C:13]1[C:22]2[C:17](=[CH:18][CH:19]=[C:20]([O:23][CH3:24])[CH:21]=2)[C:16]([C:25]2[CH:30]=[CH:29][C:28]([CH2:31]Cl)=[CH:27][CH:26]=2)=[N:15][N:14]=1>C(O)C>[Cl:12][C:13]1[C:22]2[C:17](=[CH:18][CH:19]=[C:20]([O:23][CH3:24])[CH:21]=2)[C:16]([C:25]2[CH:30]=[CH:29][C:28]([CH2:31][N:9]([CH2:10][CH3:11])[CH2:7][CH3:8])=[CH:27][CH:26]=2)=[N:15][N:14]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8021DiethylamineHCID 11430Potassium CarbonateHCID 866122301-Chloro-4-(4-chloromethylphenyl)-7-methoxyphthalazine

생성물 1

HCID 86612229HCID 86612229, 화합물수율 80%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
85 °C

실험 절차

280 mg (2 mmol) of potassium carbonate and 0.3 mL of diethylamine are added to a solution of 319 mg (1 mmol) of 1-chloro-4-(4-chloromethylphenyl)-7-methoxyphthalazine (synthesized in 30.3) in 3 mL of ethanol. The mixture is stirred at 85° C. for 4 hours. The ethanol is evaporated off and the residue is taken up in water and extracted with dichloromethane. The organic extracts are washed with brine, dried over anhydrous sodium sulfate and then evaporated under reduced pressure. The residue obtained is purified by chromatography on a column of silica gel (solvent: 95/5 to 85/15 (v/v) dichloromethane/methanol). 287 mg of product are obtained (80% yield).

후처리

  1. customThe ethanol is evaporated off
  2. extractionextracted with dichloromethane
  3. washThe organic extracts are washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customevaporated under reduced pressure
  6. customThe residue obtained
  7. customis purified by chromatography on a column of silica gel (solvent: 95/5 to 85/15 (v/v) dichloromethane/methanol)

출처 및 근거

ORD 기록
ord-cd90850b3e2f4158a1ed82648e78d21c
출처 데이터셋
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07423030B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트