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Benzoate → HCID 12017704, 화합물

HRID 1006546
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HRID 1006546 반응식
[C:1]([O-])(=O)[C:2]1C=CC=C[CH:3]=1.[C:10]1([S:16]([NH:19][C:20]2[CH:25]=[CH:24][C:23]([C:26]([F:29])([F:28])[F:27])=[CH:22][C:21]=2[NH:30][CH2:31][C:32]2[CH:41]=[CH:40][C:35]([C:36]([O:38][CH3:39])=[O:37])=[CH:34][CH:33]=2)(=[O:18])=[O:17])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[H-].[Na+].[CH3:44]I>CN(C=O)C>[CH3:44][N:30]([CH2:31][C:32]1[CH:33]=[CH:34][C:35]([C:36]([O:38][CH3:39])=[O:37])=[CH:40][CH:41]=1)[C:21]1[CH:22]=[C:23]([C:26]([F:29])([F:28])[F:27])[CH:24]=[CH:25][C:20]=1[N:19]([S:16]([C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1)(=[O:17])=[O:18])[CH:2]([CH3:3])[CH3:1]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 242BenzoateHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 22671955HCID 22671955, 화합물

생성물 1

HCID 12017704HCID 12017704, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

Methyl 4-[2-(N-isopropyl-phenylsulfonylamino)-5-trifluoromethyl-phenyl]aminomethyl]benzoate (200 mg) prepared by the same procedure as Example 17 by using methyl 4-(2-phenylsulfonylamino-5-trifluoromethyl-phenylaminomethyl)benzoate (prepared in Example 27) was dissolved in DMF (5 ml). Sodium hydride (64 mg) and methyl iodide (200 μl) were added thereto. The mixture was stirred for 24 hours at 60° C. The reaction mixture was extracted with H2O-AcOEt, washed, dried over, filtered and concentrated under the reduced pressure. The residue was purified on silica gel column chromatography (hexane:AcOEt=5:1) to give the title compound (105 mg) having the following physical data.

후처리

  1. extractionThe reaction mixture was extracted with H2O-AcOEt
  2. washwashed
  3. customdried over,
  4. filtrationfiltered
  5. concentrationconcentrated under the reduced pressure
  6. customThe residue was purified on silica gel column chromatography (hexane:AcOEt=5:1)

출처 및 근거

ORD 기록
ord-b291a97798344867b87aafa567bda363
출처 데이터셋
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06790866B2

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