Benzylamine → HCID 22903655、化合物

HRID 1489157ノート

反応式

HRID 1489157 の反応式
ON1C2C=CC=CC=2N=N1.C1(N=C=NC2CCCCC2)CCCCC1.[CH2:26]([N:33]1[C:37](=[O:38])[CH2:36][C:35]([C:44]([O-:46])=O)([C:39]([O:41][CH2:42][CH3:43])=[O:40])[CH2:34]1)[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1.[CH2:47]([NH2:54])[C:48]1[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=1>O1CCCC1>[CH2:26]([N:33]1[C:37](=[O:38])[CH2:36][C:35]([C:44](=[O:46])[NH:54][CH2:47][C:48]2[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=2)([C:39]([O:41][CH2:42][CH3:43])=[O:40])[CH2:34]1)[C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1

参加物

6

反応物 4

HCID 7504BenzylamineHCID 10868DicyclohexylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 86751384HCID 86751384、化合物

生成物 1

HCID 22903655HCID 22903655、化合物収率 99.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1-Hydroxybenztriazole (2.78 g) and dicyclohexylcarbodiimide (42.5 g) were added to a mixture of monoethyl 1-benzyl-5-oxopyrrolidine-3,3-dicarboxylate (60.0 g), benzylamine (23.2 g) and tetrahydrofuran (500 ml), and the mixture was stirred at room temperature overnight. The insoluble matter was removed by filtration and the filtrate was concentrated. Ethyl acetate (400 ml) was added and the mixture was sequentially washed with an aqueous solution of potassium carbonate, water, dilute hydrochloric acid and saturated brine, dried, and concentrated to give 78 g of the object compound as white crystals, melting point 63°-65° C.

後処理

  1. customThe insoluble matter was removed by filtration
  2. concentrationthe filtrate was concentrated
  3. additionEthyl acetate (400 ml) was added
  4. washthe mixture was sequentially washed with an aqueous solution of potassium carbonate, water, dilute hydrochloric acid and saturated brine
  5. customdried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-4a379a635a0b4a66bb9f12e491c00d19
出典データセット
uspto-grants-1997_10
特許番号
US05677316

反応ノート

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