Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) → HCID 70981105、化合物

HRID 1409332ノート

反応式

HRID 1409332 の反応式
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]2[N:8]([CH:10]=[C:11]([C:13]([OH:15])=O)[N:12]=2)[CH:9]=1)([O-:3])=[O:2].[NH2:16][C@@H:17]([CH3:34])[CH2:18][N:19]1[CH:23]=[CH:22][C:21]([C:24]2[CH:31]=[C:30]([F:32])[C:27]([C:28]#[N:29])=[C:26]([Cl:33])[CH:25]=2)=[N:20]1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C>[Cl:33][C:26]1[CH:25]=[C:24]([C:21]2[CH:22]=[CH:23][N:19]([CH2:18][C@@H:17]([NH:16][C:13]([C:11]3[N:12]=[C:7]4[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:9][N:8]4[CH:10]=3)=[O:15])[CH3:34])[N:20]=2)[CH:31]=[C:30]([F:32])[C:27]=1[C:28]#[N:29]

参加物

5

反応物 3

HCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 33949666-nitroimidazo[1,2-a]pyridine-2-carboxylic acidHCID 67170587(S)-4-(1-(2-aminopropyl)-1H-pyrazol-3-yl)-2-chloro-6-fluorobenzonitrile

生成物 1

HCID 70981105HCID 70981105、化合物収率 18.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

The title compound was prepared using the procedure described in Example 3(h) starting from 6-nitroimidazo[1,2-a]pyridine-2-carboxylic acid (0.551 mmol, 0.114 g) and (S)-4-(1-(2-aminopropyl)-1H-pyrazol-3-yl)-2-chloro-6-fluorobenzo-nitrile (0.459 mmol, 0.128 g). DMF (4 ml) was used as the solvent and HBTU (0.046 mmol, 0.017 g) was used instead of HOBt. The crude product was purified by preparative HPLC. 0.0405 g of the title compound was obtained. 1H-NMR (400 MHz, MeOH-d4): δ 1.37 (d, 3H), 4.30-4.37 (m, 1H), 4.38-4.46 (m, 1H), 4.59-4.72 (m, 1H), 6.72 (d, 1H), 7.54 (d, 1H), 7.68 (d, 1H), 7.72 (s, 1H), 7.78 (d, 1H), 8.15-8.21 (m, 1H), 8.38 (s, 1H), 10.40-10.44 (m, 1H).

後処理

  1. customThe title compound was prepared
  2. customThe crude product was purified by preparative HPLC

出典と根拠

ORDレコード
ord-2f4dc99df76c4b0ead174d75f14bcfd6
出典データセット
uspto-grants-2014_12
特許番号
US08921378B2

反応ノート

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