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

Triethylamine → Benzyl 3-(5-cyano-4-(2,6-difluorophenyl)-N-isopropyl-1H-1,2,3-triazole-1-carboxamido)benzoate

HRID 2097674
노트
인쇄 미리보기

반응식

HRID 2097674 반응식
[CH:1]([NH:4][C:5]1[CH:6]=[C:7]([CH:18]=[CH:19][CH:20]=1)[C:8]([O:10][CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=[O:9])([CH3:3])[CH3:2].C(N(CC)CC)C.ClC(Cl)(O[C:32](=[O:38])OC(Cl)(Cl)Cl)Cl.[F:40][C:41]1[CH:46]=[CH:45][CH:44]=[C:43]([F:47])[C:42]=1[C:48]1[N:49]=[N:50][NH:51][C:52]=1[C:53]#[N:54]>ClCCl.CN(C1C=CN=CC=1)C.CCOC(C)=O>[C:53]([C:52]1[N:51]([C:32]([N:4]([C:5]2[CH:6]=[C:7]([CH:18]=[CH:19][CH:20]=2)[C:8]([O:10][CH2:11][C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)=[O:9])[CH:1]([CH3:3])[CH3:2])=[O:38])[N:50]=[N:49][C:48]=1[C:42]1[C:43]([F:47])=[CH:44][CH:45]=[CH:46][C:41]=1[F:40])#[N:54]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 8471TriethylamineHCID 94429TriphosgeneHCID 58501909Benzyl 3-(isopropylamino)benzoateHCID 1785106704-(2,6-difluorophenyl)-1H-1,2,3-triazole-5-carbonitrile

생성물 1

HCID 58501889Benzyl 3-(5-cyano-4-(2,6-difluorophenyl)-N-isopropyl-1H-1,2,3-triazole-1-carboxamido)benzoate

시약·촉매·용매 3

HCID 14284
4-(Dimethylamino)pyridine
촉매
HCID 6344Dichloromethane용매
HCID 8857Ethyl Acetate용매

실험 절차

To a solution of benzyl 3-(isopropylamino)benzoate (5) in dry dichloromethane (0.4 M) under Ar at 0° C. was added triethylamine (1.5 equiv) followed by triphosgene (1.5 equiv). The resulting mixture was stirred at rt for 15 min and was concentrated in vacuo. The residue was suspended in dry toluene (0.4 M), DMAP (1.0 equiv) and 4-(2,6-difluorophenyl)-1H-1,2,3-triazole-5-carbonitrile (2) (1.0 equiv) were added and the resulting suspension was heated to reflux for 1 h, then cooled to rt, diluted with AcOEt and washed with water, 10% HCl and brine. The organic layer was dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by flash chromatography (Hexanes/AcOEt as eluant). Benzyl 3-(5-cyano-4-(2,6-difluorophenyl)-N-isopropyl-1H-1,2,3-triazole-1-carboxamido)benzoate (6) was obtained as a pale yellow foam.

후처리

  1. concentrationwas concentrated in vacuo
  2. temperaturethe resulting suspension was heated
  3. temperatureto reflux for 1 h
  4. temperaturecooled to rt
  5. washwashed with water, 10% HCl and brine
  6. dry with materialThe organic layer was dried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe residue was purified by flash chromatography (Hexanes/AcOEt as eluant)

출처 및 근거

ORD 기록
ord-76b01bf5e1bb4d20b77aa21e9aeb2d7a
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08450350B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트