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

Carbon Dioxide → N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-N'-methyl-3,4,5,6-tetrahydrophthalamide

HRID 742424
노트
인쇄 미리보기

반응식

HRID 742424 반응식
Cl.[CH3:2][NH2:3].[C:4](=[O:7])([O-])[O-].[K+].[K+].C(=O)=O.[F:13][C:14]1[CH:19]=[C:18]([Cl:20])[C:17]([O:21][CH:22]2[CH2:26][CH2:25][CH2:24][CH2:23]2)=[CH:16][C:15]=1[N:27]1[C:32](=[O:33])C2CCCC(=C2)C1=O.Cl>C(#N)C>[F:13][C:14]1[CH:19]=[C:18]([Cl:20])[C:17]([O:21][CH:22]2[CH2:23][CH2:24][CH2:25][CH2:26]2)=[CH:16][C:15]=1[NH:27][C:32](=[O:33])[C:14]1[CH2:19][CH2:18][CH2:17][CH2:16][C:15]=1[C:4]([NH:3][CH3:2])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 280Carbon DioxideHCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 6364545Methylamine hydrochlorideHCID 19425191N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-3,4,5,6-tetrahydroisophthalimide

생성물 1

HCID 19425267N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-N'-methyl-3,4,5,6-tetrahydrophthalamide
수율 107.5%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Methylamine hydrochloride (0.200 g, 2.96 mmol) and potassium carbonate (0.400 g, 2.89 mmol), and acetonitrile (5 ml) as a solvent were placed into a round bottom flask (25 cc), followed by stirring at room temperature. After confirming the generation of carbon dioxide gas, N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-3,4,5,6-tetrahydroisophthalimide (0.650 g, 1.79 mmol) was added thereto, followed by stirring overnight at room temperature. After completion of the reaction, the reaction mixture was poured into 1N hydrochloric acid (20 ml), and the mixture was extracted with ethyl acetate (40 ml×3 portions). After drying the organic layer over anhydrous magnesium sulfate, the drying agent was removed, and the solvent was distilled off under reduced pressure. The precipitated crystals were isolated by filtration, thoroughly washed with hexane and dried to obtain N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-N'-methyl-3,4,5,6-tetrahydrophthalamide as white crystals (0.380 g, 53.8% yield). The melting point and the spectral data thereof are shown in Example 37.

후처리

  1. additionwas added
  2. stirringby stirring overnight at room temperature
  3. customAfter completion of the reaction
  4. extractionthe mixture was extracted with ethyl acetate (40 ml×3 portions)
  5. dry with materialAfter drying the organic layer over anhydrous magnesium sulfate
  6. customthe drying agent was removed
  7. distillationthe solvent was distilled off under reduced pressure
  8. customThe precipitated crystals were isolated by filtration
  9. washthoroughly washed with hexane
  10. customdried

출처 및 근거

ORD 기록
ord-1b32a56387f6467387b71f463e860bc1
출처 데이터셋
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05554581

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트