1-Hydroxybenzotriazole → HCID 59483777, 화합물

HRID 1808387노트

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HRID 1808387 반응식
CCN(C(C)C)C(C)C.CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1.[C:32]([O:36][C:37]([N:39]1[CH2:44][CH2:43][N:42]2[CH:45]=[C:46]([C:48]([OH:50])=O)[N:47]=[C:41]2[CH2:40]1)=[O:38])([CH3:35])([CH3:34])[CH3:33].[N:51]1[CH:56]=[CH:55][C:54]([N:57]2[CH2:62][CH2:61][C:60]3([CH2:67][CH2:66][NH:65][CH2:64][CH2:63]3)[CH2:59][CH2:58]2)=[CH:53][CH:52]=1>C(Cl)Cl>[N:51]1[CH:52]=[CH:53][C:54]([N:57]2[CH2:62][CH2:61][C:60]3([CH2:63][CH2:64][N:65]([C:48]([C:46]4[N:47]=[C:41]5[CH2:40][N:39]([C:37]([O:36][C:32]([CH3:33])([CH3:34])[CH3:35])=[O:38])[CH2:44][CH2:43][N:42]5[CH:45]=4)=[O:50])[CH2:66][CH2:67]3)[CH2:59][CH2:58]2)=[CH:55][CH:56]=1

참가 물질

7

반응물 5

HCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 159408113-(Pyridin-4-yl)-3,9-diazaspiro[5.5]undecaneHCID 445585487-(tert-Butoxycarbonyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine-2-carboxylic acid

생성물 1

HCID 59483777HCID 59483777, 화합물수율 63%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

DIPEA (5.96 mmol, 4.0 equiv.), EDCl (2.24 mmol, 1.5 equiv.) and HOBt (2.24 mmol, 1.5 equiv.) were added at 0° C. to a solution of 7-(tert-butoxycarbonyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine-2-carboxylic acid (1.49 mmol, 1.0 equiv.) in DCM (20 ml), and the mixture was stirred for 30 min. A solution of 3-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecane (F-19) (1.49 mmol, 1.0 equiv.) in DCM (5 ml) was added at 0° C., and then the reaction mixture was stirred for 16 h at 25° C. The mixture was diluted with DCM (100 ml) and washed with sat. sodium carbonate solution (65 ml), sat. ammonium chloride solution (65 ml), water (50 ml) and sat. sodium chloride solution (50 ml), dried over Na2SO4 and concentrated in vacuo. The resulting crude product was used directly in the following stage. Yield: 63%

후처리

  1. stirringthe reaction mixture was stirred for 16 h at 25° C
  2. washwashed with sat. sodium carbonate solution (65 ml), sat. ammonium chloride solution (65 ml), water (50 ml) and sat. sodium chloride solution (50 ml)
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-c147575b3e3941c5b61aa1258834be3e
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08357717B2

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