2,4-Dichloro-6-methoxy-3,5-triazine → 4-Chloro-6-methoxy-N-{2-[4-(trifluoromethoxy)phenyl]ethyl}-1,3,5-triazin-2-amine

HRID 517483

반응식

HRID 517483 반응식
Cl[C:2]1[N:7]=[C:6]([Cl:8])[N:5]=[C:4]([O:9][CH3:10])[N:3]=1.CCN(C(C)C)C(C)C.[F:20][C:21]([F:33])([F:32])[O:22][C:23]1[CH:28]=[CH:27][C:26]([CH2:29][CH2:30][NH2:31])=[CH:25][CH:24]=1>C(#N)C>[Cl:8][C:6]1[N:5]=[C:4]([O:9][CH3:10])[N:3]=[C:2]([NH:31][CH2:30][CH2:29][C:26]2[CH:25]=[CH:24][C:23]([O:22][C:21]([F:20])([F:32])[F:33])=[CH:28][CH:27]=2)[N:7]=1

참가 물질

5

반응물 3

HCID 192672,4-Dichloro-6-methoxy-3,5-triazineHCID 81531DiisopropylethylamineHCID 106320402-[4-(Trifluoromethoxy)phenyl]ethan-1-amine

생성물 1

HCID 896196194-Chloro-6-methoxy-N-{2-[4-(trifluoromethoxy)phenyl]ethyl}-1,3,5-triazin-2-amine수율 90.5%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 5 g of 2,4-dichloro-6-methoxy-1,3,5-triazine in 50 ml of acetonitrile is cooled on an ice bath, 3.55 ml of DIPEA and then 5.13 g of 2-[4-(trifluoromethoxy)phenyl]ethanamine are added and the mixture is stirred for 30 minutes. The reaction mixture is partially concentrated under vacuum, an EtOAc/water mixture is added, the phases are separated by settling, the organic phase is washed with saturated NaCl solution and dried over MgSO4, and the solvent is evaporated off under vacuum. The precipitate formed during the evaporation is drained by suction, washed with EtOAc and dried. 7.89 g of the expected compound are obtained.

후처리

  1. concentrationThe reaction mixture is partially concentrated under vacuum
  2. additionan EtOAc/water mixture is added
  3. customthe phases are separated
  4. washthe organic phase is washed with saturated NaCl solution
  5. dry with materialdried over MgSO4
  6. customthe solvent is evaporated off under vacuum
  7. customThe precipitate formed during the evaporation
  8. washwashed with EtOAc
  9. customdried

출처 및 근거

ORD 기록
ord-db652a6b705346deb2812c9a881d2ec1
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115121B2

연결된 노트

불러오는 중…