Benzylamine → HCID 22903655, 화합물

HRID 1489157노트

반응식

HRID 1489157 반응식
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

참가 물질

6

반응물 4

HCID 7504BenzylamineHCID 10868DicyclohexylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 86751384HCID 86751384, 화합물

생성물 1

HCID 22903655HCID 22903655, 화합물수율 99.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4a379a635a0b4a66bb9f12e491c00d19
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05677316

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