Water → HCID 178441029、化合物

HRID 736373ノート

反応式

HRID 736373 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[O:21])[C:13]2[CH:18]=[CH:17][C:16]([C:19]#[N:20])=[CH:15][CH:14]=2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[N-:22]=[N+:23]=[N-:24].[Na+].[Mg+2].[Cl-].[Cl-].O>CN(C)C(=O)C>[C:1]([C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[O:21])[C:13]2[CH:14]=[CH:15][C:16]([C:19]3[NH:24][N:23]=[N:22][N:20]=3)=[CH:17][CH:18]=2)=[CH:7][CH:6]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

6

反応物 4

HCID 962WaterHCID 33557Sodium AzideHCID 2111998HCID 2111998、化合物HCID 5360315Magnesium Chloride

生成物 1

HCID 178441029HCID 178441029、化合物

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
150 °C

実験手順

The product from Example 4A (300 mg, 1.08 mmol) in N,N-dimethylacetamide (10 mL) was treated with NaN3 (0.7 g, 10.8 mmol) and MgCl2 (1.03 g, 10.8 mmol). The mixture was heated at 150° C. for 16 hours, allowed to cool to room temperature, and poured into H2O (50 mL). The mixture was filtered and the filter cake air-dried to provide the title compound as a solid. 1H NMR (300 MHz, DMSO-d6) δ 10.14 (s, 1H), 8.10 (d, J=8.4 Hz, 2H), 7.97 (d, J=8.4 Hz, 2H), 7.71 (d, J=8.5 Hz, 2H), 7.36 (d, J=8.4 Hz, 2H), 1.29 (s, 9H); MS (ESI+) m/z 322 (M+H)+.

後処理

  1. temperatureto cool to room temperature
  2. filtrationThe mixture was filtered
  3. customthe filter cake air-dried

出典と根拠

ORDレコード
ord-a6b9ce3100184e3cbc5cf499209c2922
出典データセット
uspto-grants-2009_09
特許番号
US07595332B2

反応ノート

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