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

HRID 1367910ノート

反応式

HRID 1367910 の反応式
[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]

参加物

7

反応物 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、化合物2 回

生成物 1

HCID 66940416HCID 66940416、化合物収率 40%

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide溶媒HCID 81531Diisopropylethylamine溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

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)+.

後処理

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

出典と根拠

ORDレコード
ord-9b5bc7a1c2e54686ab4a3cae85eaa5af
出典データセット
uspto-grants-2011_02
特許番号
US07893267B2

反応ノート

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