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

Methylamine → (4-Chlorophenyl)-N,N'-dimethylethanimidamide--hydrogen chloride (1/1)

HRID 437101
노트
인쇄 미리보기

반응식

HRID 437101 반응식
[CH3:1][NH:2][C:3](=O)[CH2:4][C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][CH:6]=1.F[B-](F)(F)F.C([O+](CC)CC)C.[CH3:25][NH2:26]>C(Cl)Cl>[ClH:11].[Cl:11][C:8]1[CH:9]=[CH:10][C:5]([CH2:4][C:3]([NH:26][CH3:25])=[N:2][CH3:1])=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6329MethylamineHCID 2723982Triethyloxonium tetrafluoroborateHCID 46269662-(4-chlorophenyl)-N-methylacetamide

생성물 1

HCID 3040074(4-Chlorophenyl)-N,N'-dimethylethanimidamide--hydrogen chloride (1/1)수율 17.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Using glass vessels dried at 125° C. before use, N-methyl-2-(4-chlorophenyl)acetamide (18.4 grams; 0.1 mole) is dispersed in a mixture of 150 milliliters of methylene chloride and triethyloxonium fluoroborate (19 grams; 0.1 mole). The reaction mixture is stirred at room temperature for 72 hours, then cooled in an acetone-Dry Ice bath while monomethylamine (10 grams; 0.33 mole) is added. The mixture is then stirred an additional 18 hours at room temperature. During the foregoing additions and mixing of reactants the mixture is maintained under a dry nitrogen blanket. The reaction mixture is then concentrated under vacuum and the residue is suspended in water, made strongly alkaline by addition of cold aqueous 20 percent sodium hydroxide, and extracted with ethyl acetate. The organic phase is separated and dried over anhydrous sodium sulfate. Excess dry gaseous hydrogen chloride is introduced into the mixture, and the resulting mixture is evaporated under reduced pressure, residual oil is taken up in methyl ethyl ketone, filtered and the filtrate evaporated. The product is obtained as a residue which is recrystallized from isopropanol. The 2-(4-chlorophenyl)-N,N'-dimethylacetamidine hydrochloride product is obtained in a yield of 4 grams; corresponding to a 17.1 percent yield based on the acetamide starting material. The product is found to melt at a temperature of 242.5°-243.5° C. Infrared and nuclear magnetic resonance analyses also confirm the named structure.

후처리

  1. additionis added
  2. stirringThe mixture is then stirred an additional 18 hours at room temperature
  3. additionDuring the foregoing additions and mixing of reactants the mixture
  4. temperatureis maintained under a dry nitrogen blanket
  5. concentrationThe reaction mixture is then concentrated under vacuum
  6. additionmade strongly alkaline by addition of cold aqueous 20 percent sodium hydroxide
  7. extractionextracted with ethyl acetate
  8. customThe organic phase is separated
  9. dry with materialdried over anhydrous sodium sulfate
  10. additionExcess dry gaseous hydrogen chloride is introduced into the mixture
  11. customthe resulting mixture is evaporated under reduced pressure, residual oil
  12. filtrationfiltered
  13. customthe filtrate evaporated
  14. customThe product is obtained as a residue which
  15. customis recrystallized from isopropanol

출처 및 근거

ORD 기록
ord-df48c45856e740df8534d76d057f2fae
출처 데이터셋
uspto-grants-1977_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04029703

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트