Triethylamine → HCID 67349738, 화합물

HRID 910582노트

반응식

HRID 910582 반응식
ON1C(=O)CCC1=O.C(N(CC)CC)C.Cl[C:17]([O:19][CH2:20][CH3:21])=[O:18].[CH2:22]([C:29]1[C:30](=[O:37])[NH:31][NH:32][C:33]=1[CH:34]([CH3:36])[CH3:35])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>O1CCCC1>[CH2:22]([C:29]1[C:30](=[O:37])[NH:31][N:32]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:33]=1[CH:34]([CH3:35])[CH3:36])[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 80170N-HydroxysuccinimideHCID 673516914-Benzyl-1,2-dihydro-5-isopropyl-3H-pyrazol-3-one

생성물 1

HCID 67349738HCID 67349738, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

N-Hydroxysuccinimide (1.06 g) was dissolved in tetrahydrofuran (10 g) at room temperature. Triethylamine (0.936 g) and ethyl chloroformate (1.00 g) were added to the solution successively. After stirring the reaction mixture at room temperature for 30 minutes, 4-benzyl-1,2-dihydro-5-isopropyl-3H-pyrazol-3-one (2.00 g) was added to the mixture at room temperature. After the reaction mixture was stirred at room temperature for 13 hours, the reaction mixture was stirred at 50° C. for 6 hours. The insoluble materials were removed, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=4/1) to give 4-benzyl-1-ethoxycarbonyl-1,2-dihydro-5-isopropyl-3H-pyrazol-3-one.

후처리

  1. stirringAfter the reaction mixture was stirred at room temperature for 13 hours
  2. stirringthe reaction mixture was stirred at 50° C. for 6 hours
  3. customThe insoluble materials were removed
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=4/1)

출처 및 근거

ORD 기록
ord-096bef241be745008c3f90ba77613bc3
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022192B2

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