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Triethylamine → HCID 69871576、化合物

HRID 2084991
ノート
印刷プレビュー

反応式

HRID 2084991 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 13030900HCID 13030900、化合物HCID 22728596HCID 22728596、化合物

生成物 1

HCID 69871576HCID 69871576、化合物

試薬・触媒・溶媒

2
HCID 8857Ethyl Acetate溶媒HCID 12051Diethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-84bf6c7487244107b05592ed24f7cb8b
出典データセット
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06719520B2

反応ノート

読み込み中…

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