1,2-Dichloroethane → HCID 66571517, 화합물

HRID 83660노트

반응식

HRID 83660 반응식
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][N:7]2[CH:11]=[CH:10][N:9]=[C:8]2[C:12]([OH:14])=O)=[CH:4][CH:3]=1.CCN(C(C)C)C(C)C.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.Cl.[CH2:41]([NH:48][C:49]([CH:51]1[CH2:56][CH2:55][NH:54][CH2:53][CH2:52]1)=[O:50])[C:42]1[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1>O.CN(C=O)C>[CH2:41]([NH:48][C:49]([CH:51]1[CH2:56][CH2:55][N:54]([C:12]([C:8]2[N:7]([CH2:6][C:5]3[CH:4]=[CH:3][C:2]([Cl:1])=[CH:16][CH:15]=3)[CH:11]=[CH:10][N:9]=2)=[O:14])[CH2:53][CH2:52]1)=[O:50])[C:42]1[CH:43]=[CH:44][CH:45]=[CH:46][CH:47]=1

참가 물질

8

반응물 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 16232225N-benzylpiperidine-4-carboxamide hydrochlorideHCID 683797411-[(4-Chlorophenyl)methyl]-1H-imidazole-2-carboxylic acid

생성물 1

HCID 66571517HCID 66571517, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

The following was added sequentially to DMF: 1-(4-chlorobenzyl)-1H-imidazole-2-carboxylic acid (71 mg, 0.298 mmol), DIPEA (0.16 mL, 0.894 mmol), EDC (69 mg, 0.358 mmol), and HOBT (55 mg, 0.358 mmol). This was allowed to stir at rt for 30 min, at which time N-benzylpiperidine-4-carboxamide hydrochloride (76 mg, 0.298 mmol) was added and stirring continued at rt for 14 h. Addition of water caused precipitation, which was collected over a filter and washed with water and small amount of diethyl ether and EtOAc to give the title compound as a white solid. (Yield: 37 mg, 0.085 mmol, 28%) 1H NMR (400 MHz, CDCl3) 7.34-7.23, 7.13, 7.11, 7.04, 6.93, 5.79-5.65, 5.36, 4.63, 4.43, 3.14, 2.82, 2.42-2.32, 1.95, 1.83, 1.70-1.59

후처리

  1. additionwas added
  2. customprecipitation, which
  3. customwas collected over
  4. filtrationa filter
  5. washwashed with water and small amount of diethyl ether and EtOAc

출처 및 근거

ORD 기록
ord-2d9fdd34cda945b3a3a9a6598629780d
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846684B2

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