Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) → HCID 66940416, 화합물

HRID 1367910노트

반응식

HRID 1367910 반응식
[CH3:1][O:2][C:3]1[C:4]2[N:5]([CH:9]=[C:10](C(O)=O)[N:11]=2)[CH:6]=[CH:7][CH:8]=1.CN([C:18]([O:22]N1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[NH:39]1[CH:43]=[CH:42][N:41]=[C:40]1[NH:44][C:45]([C:47]1[C:55]2[NH:54][C:53]([NH2:56])=[N:52][C:51]=2[CH:50]=[CH:49][CH:48]=1)=[O:46]>CN(C=O)C.CCN(C(C)C)C(C)C.[Cl-].[Na+].O>[NH:41]1[CH:42]=[CH:43][N:39]=[C:40]1[NH:44][C:45]([C:47]1[C:55]2[N:54]=[C:53]([NH:56][C:18]([C:9]3[N:5]4[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[C:4]4=[N:11][CH:10]=3)=[O:22])[NH:52][C:51]=2[CH:50]=[CH:49][CH:48]=1)=[O:46]

참가 물질

7

반응물 3

HCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 669402468-Methoxyimidazo[1,2-A]pyridine-2-carboxylic acidHCID 178508178HCID 178508178, 화합물2회

생성물 1

HCID 66940416HCID 66940416, 화합물수율 40%

시약·촉매·용매 3

HCID 6228Dimethylformamide용매HCID 81531Diisopropylethylamine용매HCID 57417360Sodium chloride; water용매

실험 절차

300 mg (3.0 mmol) of the above 8-methoxy-imidazo[1,2-a]pyridine-2-carboxylic acid and 200 mg (0.5 mmol) of HBTU in a mixture of 1.5 mL of DMF and 0.6 mL of DIEA was reacted with 60 mg (0.25 mmol) of the 2-amino-3H-benzoimidazole-4-carboxylic acid (1H-imidazol-2-yl)-amide (Intermediate B) as described in general procedure A. After the reaction was complete, it was diluted with brine (20 mL), and the resulting solid was filtered, washed with water, ethyl acetate and dried under vacuum to give 41 mg (40%) of 2-[(8-methoxy-imidazo[1,2-a]pyridine-3-carbonyl)-amino]-1H-benzoimidazole-4-carboxylic acid (1H-imidazol-2-yl)-amide as a solid. LCMS: 417 (M+1)+.

후처리

  1. filtrationthe resulting solid was filtered
  2. washwashed with water, ethyl acetate
  3. customdried under vacuum

출처 및 근거

ORD 기록
ord-9b5bc7a1c2e54686ab4a3cae85eaa5af
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07893267B2

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