Water → HCID 59520476, 화합물

HRID 1162785노트

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HRID 1162785 반응식
[F:1][C:2]([F:11])([F:10])[C:3]1[C:7]([CH:8]=[O:9])=[CH:6][NH:5][N:4]=1.Cl[CH2:13][CH2:14][C:15]([NH:17][C:18]1[S:22][C:21]2[CH2:23][CH2:24][CH2:25][CH2:26][C:20]=2[C:19]=1[C:27]([NH:29][CH3:30])=[O:28])=[O:16].C(=O)([O-])[O-].[K+].[K+].O>CN(C=O)C.[I-].[K+]>[CH:8]([C:7]1[C:3]([C:2]([F:1])([F:10])[F:11])=[N:4][N:5]([CH2:13][CH2:14][C:15]([NH:17][C:18]2[S:22][C:21]3[CH2:23][CH2:24][CH2:25][CH2:26][C:20]=3[C:19]=2[C:27]([NH:29][CH3:30])=[O:28])=[O:16])[CH:6]=1)=[O:9]

참가 물질

7

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 59520509HCID 59520509, 화합물HCID 178519884HCID 178519884, 화합물

생성물 1

HCID 59520476HCID 59520476, 화합물수율 85%

시약·촉매·용매 2

HCID 4875Potassium Iodide촉매HCID 6228Dimethylformamide용매

실험 절차

3-(Trifluoromethyl)-1H-pyrazole-4-carbaldehyde (437 mg, 2.66 mmol) and 2-(3-chloropropanamido)-N-methyl-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxamide (801 mg, 2.66 mmol) were dissolved in DMF (15 mL). Potassium carbonate (368 mg, 2.66 mmol) was added followed by potassium iodide (10 mg, 0.06 mmol). The reaction mixture was left to stand for 7 days. Water was added and the reaction mixture extracted into EtOAc (×3). The EtOAc layers were combined and washed with water (×5), brine, dried over MgSO4, filtered and the solvent removed in vacuo to give desired product as a yellow solid (970 mg, 2.26 mmol, 85%).

후처리

  1. waitThe reaction mixture was left
  2. extractionthe reaction mixture extracted into EtOAc (×3)
  3. washwashed with water (×5), brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-6a649ba15a874ff8b729c84934ea087a
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07820707B2

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