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Ethyl Acetate → HCID 67074115, 화합물

HRID 2042693
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인쇄 미리보기

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HRID 2042693 반응식
[NH2:1][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.CCN(C(C)C)C(C)C.Cl[C:20]1[N:25]=[C:24]([O:26][CH2:27][C:28]([F:31])([F:30])[F:29])[N:23]=[C:22]([NH:32][C:33]2[CH:42]=[CH:41][C:36]([C:37]([O:39][CH3:40])=[O:38])=[CH:35][CH:34]=2)[N:21]=1.CCOC(C)=O>C1COCC1>[OH:9][C:6]1[CH:7]=[CH:8][C:3]([CH2:2][NH:1][C:20]2[N:25]=[C:24]([O:26][CH2:27][C:28]([F:31])([F:29])[F:30])[N:23]=[C:22]([NH:32][C:33]3[CH:42]=[CH:41][C:36]([C:37]([O:39][CH3:40])=[O:38])=[CH:35][CH:34]=3)[N:21]=2)=[CH:4][CH:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 81531DiisopropylethylamineHCID 974724-HydroxybenzylamineHCID 86652469Methyl 4-(4-chloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-ylamino)benzoate

생성물 1

HCID 67074115HCID 67074115, 화합물수율 75.4%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

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온도
70 °C

실험 절차

4-(aminomethyl)phenol (2.4 g) white solid and iPr2NEt (5.0 g) were added into a solution of methyl 4-(4-chloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-ylamino)benzoate (7.0 g) in THF (150 mL). The mixture was heated at 70° C. for 16 hours. After cooling, the mixture was charged with 250 mL of EtOAc. The resulting solution was washed with water (2×50 mL) and brine (30 mL). The organic layer was dried over MgSO4 and concentrated under vacuum to give a residue which was recrystallized in EtOAc to give 6.54 g of methyl 4-(4-(4-hydroxybenzylamino)-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-ylamino)benzoate.

후처리

  1. temperatureAfter cooling
  2. washThe resulting solution was washed with water (2×50 mL) and brine (30 mL)
  3. dry with materialThe organic layer was dried over MgSO4
  4. concentrationconcentrated under vacuum
  5. customto give a residue which
  6. customwas recrystallized in EtOAc

출처 및 근거

ORD 기록
ord-5287bff0b9d943b18a31cbef4587c9c9
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08586584B2

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