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Acetamide → HCID 90034137, 화합물

HRID 56257
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HRID 56257 반응식
[F:1][C:2]1[CH:3]=[C:4]([NH:14][C:15](=[O:28])[CH2:16][C:17](=O)[CH2:18][O:19][C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([F:26])[CH:21]=2)[CH:5]=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][O:11][CH2:10][CH2:9]1.[C:29]([NH2:32])(=O)[CH3:30].C1(C)C=CC=CC=1.[NH4+].[Cl-]>C1(C)C(C)=CC=CC=1.C([O-])(C)C.C([O-])(C)C.C([O-])(C)C.C([O-])(C)C.[Ti+4]>[F:1][C:2]1[CH:3]=[C:4]([N:14]2[C:15](=[O:28])[CH:16]=[C:17]([CH2:18][O:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([F:26])[CH:21]=3)[N:32]=[C:29]2[CH3:30])[CH:5]=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][O:11][CH2:10][CH2:9]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 178AcetamideHCID 1140TolueneHCID 25517Ammonium ChlorideHCID 90022866HCID 90022866, 화합물

생성물 1

HCID 90034137HCID 90034137, 화합물수율 17%

시약·촉매·용매 2

HCID 11026Titanium isopropoxide촉매
HCID 7237
O-Xylene
용매

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온도
165 °C

실험 절차

A mixture of N-(3-fluoro-4-morpholinophenyl)-4-(3-fluorophenoxy)-3-oxobutanamide (510 mg, 1.31 mmol), acetamide (154 mg, 2.61 mmol) and titanium tetraisopropanolate (3.2 mL) in xylene (10 mL) was stirred at 165° C. for 24 h. The mixture was cooled to rt and 60 mL of toluene and 60 mL of saturated NH4Cl aqueous solution were added. The resulting mixture was stirred at rt overnight. The mixture was then filtered and the filtrate was extracted with DCM (20 mL×4). The combined organic phases were washed with brine (30 mL×2), dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=1:1) to give the title compound as a yellow solid (0.09 g, 17%). The compound was characterized by the following spectroscopic data:

후처리

  1. temperatureThe mixture was cooled to rt
  2. stirringThe resulting mixture was stirred at rt overnight
  3. filtrationThe mixture was then filtered
  4. extractionthe filtrate was extracted with DCM (20 mL×4)
  5. washThe combined organic phases were washed with brine (30 mL×2)
  6. dry with materialdried over anhydrous Na2SO4
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=1:1)

출처 및 근거

ORD 기록
ord-7f94b84019aa46418f584cd9e738e261
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09434695B2

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