Triethylamine → HCID 67349738、化合物

HRID 910582ノート

反応式

HRID 910582 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 67349738HCID 67349738、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-096bef241be745008c3f90ba77613bc3
出典データセット
uspto-grants-2011_09
特許番号
US08022192B2

反応ノート

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