1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 57665017, 화합물

HRID 1717304노트

반응식

HRID 1717304 반응식
[CH:1]1([CH2:7][C:8]2[N:12]([C:13]3[CH:18]=[CH:17][C:16]([C:19]([NH:21][CH2:22][CH3:23])=[O:20])=[CH:15][CH:14]=3)[N:11]=[N:10][C:9]=2[C:24]([OH:26])=O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C1C=C[C:30]2N(O)N=[N:33][C:31]=2[CH:32]=1.C1(N)CC1.CCN=C=NCCCN(C)C>C(#N)C.CN(C=O)C.C(=O)([O-])O.[Na+].O>[CH:1]1([CH2:7][C:8]2[N:12]([C:13]3[CH:14]=[CH:15][C:16]([C:19]([NH:21][CH2:22][CH3:23])=[O:20])=[CH:17][CH:18]=3)[N:11]=[N:10][C:9]=2[C:24]([NH:33][CH:31]2[CH2:32][CH2:30]2)=[O:26])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

참가 물질

8

반응물 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 69828CyclopropylamineHCID 757711-HydroxybenzotriazoleHCID 68513203HCID 68513203, 화합물

생성물 1

HCID 57665017HCID 57665017, 화합물수율 183.6%

시약·촉매·용매 3

HCID 962Water용매HCID 516892Sodium Bicarbonate용매HCID 21891449acetonitrile N,N-dimethylformamide용매

실험 절차

5-(Cyclohexylmethyl)-1-{4-[(ethylamino)carbonyl]phenyl}-1H-1,2,3-triazole-4-carboxylic acid (357 mg, 1.00 mmol) obtained in Example 102b), HOBt (68.2 mg, 0.500 mmol, 0.5 eq.) and cyclopropylamine (0.093 ml, 1.30 mmol, 1.3 eq.) were dissolved in acetonitrile-DMF (2:1, 4.5 ml), WSC (215 mg, 1.10 mmol, 1.1 eq.) was added, and the mixture was stirred at room temperature for 14 hr. Water was added to the reaction mixture, and the obtained suspension was diluted with 2% aqueous sodium hydrogen carbonate solution. The precipitate was collected by filtration, washed with water and dried to give the title compound as a white powder (363 mg, 0.918 mmol, 91.8%).

후처리

  1. filtrationThe precipitate was collected by filtration
  2. washwashed with water
  3. customdried

출처 및 근거

ORD 기록
ord-df5c375ef883454ebe22f0ea1228dee6
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803822B2

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