1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → HCID 131731010、化合物

HRID 2035550ノート

反応式

HRID 2035550 の反応式
[CH2:1]([NH:8][C:9]1[CH:14]=[C:13]([N:15]([CH2:28][C:29]2[CH:34]=[CH:33][C:32]([O:35][CH3:36])=[CH:31][CH:30]=2)[C:16]2[CH:17]=[N:18][C:19]([N:22]3[CH2:27][CH2:26][O:25][CH2:24][CH2:23]3)=[CH:20][CH:21]=2)[N:12]=[CH:11][C:10]=1C(O)=O)C1C=CC=CC=1.Cl.[CH2:41]([N:43]=C=NCCCN(C)C)[CH3:42].[OH2:52].ON1[C:58]2[CH:59]=[CH:60][CH:61]=[CH:62][C:57]=2N=N1.O.N>ClCCl.O>[CH2:1]([NH:8][C:9]1[CH:14]=[C:13]([N:15]([CH2:28][C:29]2[CH:34]=[CH:33][C:32]([O:35][CH3:36])=[CH:31][CH:30]=2)[C:16]2[CH:17]=[N:18][C:19]([N:22]3[CH2:27][CH2:26][O:25][CH2:24][CH2:23]3)=[CH:20][CH:21]=2)[N:12]=[CH:11][C:10]=1[CH2:42][C:41]([NH2:43])=[O:52])[C:57]1[CH:62]=[CH:61][CH:60]=[CH:59][CH:58]=1

参加物

7

反応物 4

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 12896473Azane;hydrateHCID 674139734-Benzylamino-6-[4-methoxybenzyl-(6-morpholinopyridin-3-yl)amino]pyridine-3-carboxylic acid

生成物 1

HCID 131731010HCID 131731010、化合物収率 86.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

3.4 mg of 4-benzylamino-6-[4-methoxybenzyl-(6-morpholinopyridin-3-yl)amino]pyridine-3-carboxylic acid was dissolved in 1 mL of dichloromethane, to which 1.9 mg of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride and 1.5 mg of 1-hydroxybenzotriazole monohydrate were added, and stirred at room temperature for 30 minutes. Then, 1 mL of 28% ammonia water was added, and stirred at the same temperature for 3 hours. To the reaction mixture water was added, extracted with chloroform, the extract was washed with saturated saline, and dried on anhydrous sodium sulfate. The solvent was evaporated to obtain 3.0 mg of the title compound containing impurities as a brown solid. Without further purification, this was used in the next reaction as it was.

後処理

  1. additionwere added
  2. stirringstirred at the same temperature for 3 hours
  3. extractionextracted with chloroform
  4. washthe extract was washed with saturated saline
  5. dry with materialdried on anhydrous sodium sulfate
  6. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-747b026ed676487c8e2dfc62e2928c1c
出典データセット
uspto-grants-2013_11
特許番号
US08575153B2

反応ノート

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