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

Dimethylamine → 3-[4-chloro-2-fluoro-5-(phenylmethoxy)-phenyl]-6-(dimethylamino)-1-methyl-1,3,5-triazine-2,4(1H,3H)-dione

HRID 1450167
노트
인쇄 미리보기

반응식

HRID 1450167 반응식
C(O[C:4]([N:6]([CH3:12])[C:7]([NH:10]C)=[N:8][CH3:9])=[O:5])C.[Cl:13][C:14]1[C:19]([O:20]CC2C=CC=CC=2)=[CH:18][C:17]([N:28]=[C:29]=[O:30])=[C:16]([F:31])[CH:15]=1.[CH3:32]NC.[C:35]1([CH3:41])[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1>C[O-].[Na+]>[Cl:13][C:14]1[C:19]([O:20][CH2:41][C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)=[CH:18][C:17]([N:28]2[C:29](=[O:30])[N:10]=[C:7]([N:8]([CH3:32])[CH3:9])[N:6]([CH3:12])[C:4]2=[O:5])=[C:16]([F:31])[CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 674DimethylamineHCID 1140Toluene4회HCID 199752544-Chloro-2-fluoro-5-(phenylmethoxy)phenyl isocyanateHCID 45122948N-ethoxycarbonyl-N,N', N"-trimethylguanidine

생성물 1

HCID 199752643-[4-chloro-2-fluoro-5-(phenylmethoxy)-phenyl]-6-(dimethylamino)-1-methyl-1,3,5-triazine-2,4(1H,3H)-dione

시약·촉매·용매 1

HCID 10942334
Sodium Methoxide
촉매

실험 절차

To a solution of 5.05 g (29.2 mmol) of N-ethoxycarbonyl-N,N', N"-trimethylguanidine in 25 mL of toluene was added a solution of 7.72 g (27.8 mmol) of 4-chloro-2-fluoro-5-(phenylmethoxy)phenyl isocyanate in 50 mL of toluene over a period of 30 min while maintaining the temperature between 55° C. and 80° C. It was then stirred at the same temperature for an hour. To a solution of the resulting N-[N-[4-chloro-2-fluoro-5-(phenylmethoxy) phenyl]carbamoyl-N',N'-dimethylamidino]-N-methylcarbamate in toluene was added 3.21 g (71.5 mmol) of dimethylamine in 10 mL of toluene at room temperature. While the temperature was between 25° C. and 40° C., 45 mg (0.834 mmol) of sodium methoxide was added. After 30 min, it was quenched with 100 mL of water. The aqueous layer was extracted with ethyl acetate. The combined organic layers were washed with 0.1N hydrochloric acid, brine, and water, dried (MgSO4) and concentrated in vacuo. The crude product was flash chromatographed over silica gel eluting with a 1:1 v:v mixture of ethyl acetate and hexane to give 5.3 g of the title compound as a brown solid, m.p.: 193°-194° C.; 1H-NMR (CDCl3, 200 MHZ) ppm 7.4 (m, 6H), 6.95 (d, 1H), 5.05 (d, 2H), 3.45 (s, 3H), 3.1 (s, 6H).

후처리

  1. temperaturewhile maintaining the temperature between 55° C. and 80° C
  2. customwas between 25° C. and 40° C.
  3. customit was quenched with 100 mL of water
  4. extractionThe aqueous layer was extracted with ethyl acetate
  5. washThe combined organic layers were washed with 0.1N hydrochloric acid, brine, and water
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated in vacuo
  8. customchromatographed over silica gel eluting with a 1:1 v
  9. additionv mixture of ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-0dd4c6ba757a4f4eb296ba3f8406f796
출처 데이터셋
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05602077

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트