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Triethylamine → HCID 69871576, 화합물

HRID 2084991
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HRID 2084991 반응식
C(N(CC)CC)C.O[C:9]([CH2:11][CH2:12][C:13]1[CH:18]=[CH:17][C:16]([NH:19][C:20]2[C:21](=[O:35])[NH:22][C:23](=[O:34])[C:24]=2[C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([N+:31]([O-:33])=[O:32])[CH:26]=2)=[CH:15][CH:14]=1)=[O:10].Cl.[NH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][NH:44][C:45](=[O:47])[CH3:46].Cl.CN(C)CCCN=C=NCC.ON1C2C=CC=CC=2N=N1>C(N(CC)C=O)C.C(OCC)(=O)C>[C:45]([NH:44][CH2:43][CH2:42][CH2:41][CH2:40][CH2:39][CH2:38][NH:37][C:9]([CH2:11][CH2:12][C:13]1[CH:14]=[CH:15][C:16]([NH:19][C:20]2[C:21](=[O:35])[NH:22][C:23](=[O:34])[C:24]=2[C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([N+:31]([O-:33])=[O:32])[CH:26]=2)=[CH:17][CH:18]=1)=[O:10])(=[O:47])[CH3:46]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 13030900HCID 13030900, 화합물HCID 22728596HCID 22728596, 화합물

생성물 1

HCID 69871576HCID 69871576, 화합물

시약·촉매·용매

2
HCID 8857Ethyl Acetate용매HCID 12051Diethylformamide용매

실험 절차

A solution of triethylamine (81 mg, 0.8 mmol) in dry N,N-diethylformamide (5 mL) was added to a mixture of 3-[4-[2-(hydroxycarbonyl)ethyl]phenylamino]-4-(3-nitrophenyl)-1H-pyrrole-2,5-dione (Example A763, 152 mg, 0.4 mmol), N-(6-aminohexyl)acetamide hydrochloride (78 mg, 0.4 mmol), 1-(3-dimethylamino-propyl)-3-ethylcarbodiimide hydrochloride (77 mg, 0.4 mmol) and 1-hydroxybenzotriazole (54 mg, 0.4 mmol) and the resulting mixture stirred at room temperature for 18 hours. The mixture was diluted with ethyl acetate (25 mL) and washed successively with water (2×25 mL), saturated aqueous sodium bicarbonate solution (25 mL), water (2×25 mL), brine (25 mL), dried over magnesium sulphate and concentrated. The residue was redissolved in dichloromethane-methanol (1:1 v/v), filtered and evaporated to afford the title compound as a foam.

후처리

  1. washwashed successively with water (2×25 mL), saturated aqueous sodium bicarbonate solution (25 mL), water (2×25 mL), brine (25 mL)
  2. dry with materialdried over magnesium sulphate
  3. concentrationconcentrated
  4. dissolutionThe residue was redissolved in dichloromethane-methanol (1:1 v/v)
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-84bf6c7487244107b05592ed24f7cb8b
출처 데이터셋
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06719520B2

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