Potassium Acetate → HCID 178494125, 화합물

HRID 706002노트

반응식

HRID 706002 반응식
Cl.[Cl:2][C:3]1[CH:20]=[CH:19][C:6]([O:7][C:8]2[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][C:16](=[NH:18])[NH2:17])=[CH:10][CH:9]=2)=[CH:5][C:4]=1[C:21]([F:24])([F:23])[F:22].[OH:25][CH:26]=[C:27]([CH2:32][C:33]1[CH:34]=[N:35][C:36]([O:39][CH3:40])=[N:37][CH:38]=1)[C:28](OC)=O.C([O-])(=O)C.[K+]>C1(C)C=CC=CC=1>[Cl:2][C:3]1[CH:20]=[CH:19][C:6]([O:7][C:8]2[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][C:16]3[NH:17][CH:28]=[C:27]([CH2:32][C:33]4[CH:34]=[N:35][C:36]([O:39][CH3:40])=[N:37][CH:38]=4)[C:26](=[O:25])[N:18]=3)=[CH:10][CH:9]=2)=[CH:5][C:4]=1[C:21]([F:22])([F:23])[F:24]

참가 물질

5

반응물 3

HCID 517044Potassium AcetateHCID 67773588Methyl 3-hydroxy-2-((2-methoxypyrimidin-5-yl)methyl)acrylateHCID 677756383-(4-(4-Chloro-3-(trifluoromethyl)phenoxy)phenyl)propanimidamide hydrochloride

생성물 1

HCID 178494125HCID 178494125, 화합물수율 42.3%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

The suspension of 3-(4-(4-chloro-3-(trifluoromethyl)phenoxy)phenyl)propanimidamide hydrochloride (5.9 g, 15.56 mmol), methyl 3-hydroxy-2-((2-methoxypyrimidin-5-yl)methyl)acrylate (3.49 g, 15.56 mmol) and potassium acetate (4.58 g, 46.7 mmol) in toluene (100 mL) was heated under reflux overnight. Dean-Stark apparatus was used to remove water formed in the reaction. The residue was recrystallized in ethyl acetate and washed with ether to provide the title compound (3.4 g, 42%). LCMS: rt=1.71 min, [M+H+]=517

후처리

  1. temperaturewas heated
  2. temperatureunder reflux overnight
  3. customto remove water
  4. customformed in the reaction
  5. customThe residue was recrystallized in ethyl acetate
  6. washwashed with ether

출처 및 근거

ORD 기록
ord-aa43a47642d940aba5bc945523f33e5b
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09174968B2

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