Sodium hydride → HCID 86612915, 화합물

HRID 1445888

반응식

HRID 1445888 반응식
[H-].[Na+].[CH2:3]([O:10][C:11](=[O:24])[CH2:12][O:13][C:14]1[CH:22]=[CH:21][CH:20]=[C:19]2[C:15]=1[CH:16]=[C:17]([CH3:23])[NH:18]2)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[Br:25][CH:26](Br)[CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH3:37]>CN(C=O)C.C(OCC)(=O)C>[CH2:3]([O:10][C:11](=[O:24])[CH2:12][O:13][C:14]1[CH:22]=[CH:21][CH:20]=[C:19]2[C:15]=1[CH:16]=[C:17]([CH3:23])[N:18]2[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33][CH2:32][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][Br:25])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

참가 물질

6

반응물 3

HCID 24758Sodium hydrideHCID 113249061,1-DibromododecaneHCID 58765424(2-Methyl-1H-indol-4-yloxy)-acetic acid benzyl ester

생성물 1

HCID 86612915HCID 86612915, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a suspension of sodium hydride (60% in mineral oil, 0.093 g, 6.45 mmole) in DMF (10 mL), (2-methyl-1H-indol-4-yloxy)-acetic acid benzyl ester (2) (0.845 g, 2.3 mmole) was added. The mixture was stirred at room temperature for 1 h. To the mixture, dibromododecane (0.765 g, 2.3 mmole) was added and the reaction mixture was stirred at room temperature for 18 h. The reaction was diluted with ethyl acetate and washed with water. The organic layer was separated, dried with sodium sulphate and concentrated. The residue was purified by column chromatography (10:1, hexane: EtOAc) to afford intermediate 3. Yield: 0.708 g, 45%.

후처리

  1. additionwas added
  2. stirringthe reaction mixture was stirred at room temperature for 18 h
  3. washwashed with water
  4. customThe organic layer was separated
  5. dry with materialdried with sodium sulphate
  6. concentrationconcentrated
  7. customThe residue was purified by column chromatography (10:1, hexane: EtOAc)

출처 및 근거

ORD 기록
ord-e4ca5912b9f34cb28c09fa906118453e
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07666898B2

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