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

Hydrochloric Acid → 1-Fluoro-2,2-dimethyl-4-(1,2,4-triazol-1-yl)-pentan-3-one hydrochloride

HRID 986713
노트
인쇄 미리보기

반응식

HRID 986713 반응식
[F:1][CH2:2][C:3]([CH3:13])([CH3:12])[C:4](=[O:11])[CH2:5][N:6]1[CH:10]=[N:9][CH:8]=[N:7]1.[OH-].[K+].[CH3:16]I.[ClH:18]>CS(C)=O.O>[ClH:18].[F:1][CH2:2][C:3]([CH3:13])([CH3:12])[C:4](=[O:11])[CH:5]([N:6]1[CH:10]=[N:9][CH:8]=[N:7]1)[CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 14797Potassium HydroxideHCID 127695394-Fluoro-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one

생성물 1

HCID 201559301-Fluoro-2,2-dimethyl-4-(1,2,4-triazol-1-yl)-pentan-3-one hydrochloride수율 72%

시약·촉매·용매 2

HCID 679
Dimethyl Sulfoxide
용매
HCID 962Water용매2회

실험 절차

37.2 g (0.2 mol) of 1-fluoro-2,2-dimethyl-4-(1,2,4-triazol-1-yl)-butan-3-one were dissolved in 200 ml of dimethylsulphoxide, 11.2 g (0.2 mol) of potassium hydroxide, dissolved in 24 ml of water, were added and 28.4 g (0.2 mol) of methyl iodide were added dropwise at 20° C., whilst cooling. The reaction mixture was subsequently stirred at room temperature for 24 hours and poured onto 1,000 ml of water, the mixture was extracted twice with 200 ml of methylene chloride each time, the combined organic phases were washed five times with 100 ml of water each time and dried over sodium sulphate, the solvent was distilled off, the residue was taken up in 100 ml of acetone, the mixture was filtered and the solvent was distilled off from the mother liquor. The residue was taken up in 150 ml of ethyl acetate, and 14.4 g (0.2 mol) of hydrogen chloride were passed in. Thereafter, the mixture was allowed to crystallise out. 33.8 g (72% of theory) of 1-fluoro-2,2-dimethyl-4-(1,2,4-triazol-1-yl)-pentan-3-one hydrochloride of melting point 142° C. were obtained. ##STR62##

후처리

  1. additionwere added
  2. temperaturewhilst cooling
  3. extractionthe mixture was extracted twice with 200 ml of methylene chloride each time
  4. washthe combined organic phases were washed five times with 100 ml of water each time
  5. dry with materialdried over sodium sulphate
  6. distillationthe solvent was distilled off
  7. filtrationthe mixture was filtered
  8. distillationthe solvent was distilled off from the mother liquor
  9. customto crystallise out

출처 및 근거

ORD 기록
ord-6205ab5362be4bfb9d2caf79a0914b04
출처 데이터셋
uspto-grants-1987_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04715887

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트