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

Triethylamine → HCID 53734757, 화합물

HRID 2187612
노트
인쇄 미리보기

반응식

HRID 2187612 반응식
[NH2:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH:3]=1.[F:19][C:20]1[CH:25]=[CH:24][C:23]([C:26](=O)[CH2:27][N:28]2[CH:32]=[CH:31][N:30]=[CH:29]2)=[CH:22][CH:21]=1.C(N(CC)CC)C.C([BH3-])#N.[Na+].C(=O)([O-])O.[Na+]>ClCCl.CO.[Cl-].[Ti+4].[Cl-].[Cl-].[Cl-]>[F:19][C:20]1[CH:25]=[CH:24][C:23]([CH:26]([NH:1][C:2]2[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([C:12]3[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=3)[CH:3]=2)[CH2:27][N:28]2[CH:32]=[CH:31][N:30]=[CH:29]2)=[CH:22][CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 5003444Sodium cyanoborohydrideHCID 51512791-(4-fluorophenyl)-2-(1H-imidazol-1-yl)ethan-1-oneHCID 18476027HCID 18476027, 화합물

생성물 1

HCID 53734757HCID 53734757, 화합물수율 52%

시약·촉매·용매

3
HCID 160960Diamminetetrachlorotitanate(IV)촉매HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

Titanium chloride (2.86 ml; 26 mmol) was added portionwise to a solution of methyl 4-amino-2-(4-fluorophenyl)benzoate (5 g; 20 mmol), 1-(4-fluorophenyl)-2-(imidazol-1-yl) ethanone (4.08 g; 20 mmol) and triethylamine (8.4 ml; 60 mmol) in dichloromethane (120 ml) at 0° C. under argon atmosphere. After stirring overnight at ambient temperature, sodium cyanoborohydride (1.4 g; 0.22 mmol) in solution in methanol (10 ml) was added at 0° C. The reaction mixture was stirred for 2 hours at ambient temperature, treated with 5% aqueous sodium hydrogen carbonate solution, filtered and extracted with dichloromethane. After evaporation to dryness of the organic phase, the residue was purified by flash chromatography eluting with dichloromethane/ethanol 95/5 to give methyl 4-[1-(4-fluorophenyl)-2-(imidazol-1-yl)ethylamino]-2-(4-fluorophenyl)benzoate. Yield 52%.

후처리

  1. stirringThe reaction mixture was stirred for 2 hours at ambient temperature
  2. filtrationfiltered
  3. extractionextracted with dichloromethane
  4. customAfter evaporation to dryness of the organic phase
  5. customthe residue was purified by flash chromatography
  6. washeluting with dichloromethane/ethanol 95/5

출처 및 근거

ORD 기록
ord-df3c8ec8df954fa1aee550a7315bab36
출처 데이터셋
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06410539B1

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트