Ammonium Chloride → HCID 178433654、化合物

HRID 2234006ノート

反応式

HRID 2234006 の反応式
[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([CH3:8])[NH:4][C:3]=1[C:9]([NH:11][CH:12]1[CH2:17][CH2:16][N:15]([C:18]2[S:19][C:20]([C:23]#[N:24])=[CH:21][N:22]=2)[CH2:14][CH2:13]1)=[O:10].[N-:25]=[N+:26]=[N-:27].[Na+].[Cl-].[NH4+]>CN(C=O)C>[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([CH3:8])[NH:4][C:3]=1[C:9]([NH:11][CH:12]1[CH2:17][CH2:16][N:15]([C:18]2[S:19][C:20]([C:23]3[NH:27][N:26]=[N:25][N:24]=3)=[CH:21][N:22]=2)[CH2:14][CH2:13]1)=[O:10]

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 68580052HCID 68580052、化合物

生成物 1

HCID 178433654HCID 178433654、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
120 °C

実験手順

To a solution of 3,4-dichloro-N-[1-(5-cyano-1,3-thiazol-2-yl)piperidin-4-yl]-5-methyl-1H-pyrrole-2-carboxamide (Example 321, 0.100 g, 0.26 mmol) in DMF (3 ml) was added sodium azide (0.169 g, 2.60 mmol) followed by the addition of ammonium chloride (0.139 g, 2.60 mmol) at room temperature. The reaction was stirred at 120° C. for 3 hrs. The reaction mixture was cooled to room temperature, filtered and purified by reverse phase HPLC eluting with acetonitrile/water (0.1% TFA) (0.025 g).

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. filtrationfiltered
  3. custompurified by reverse phase HPLC
  4. washeluting with acetonitrile/water (0.1% TFA) (0.025 g)

出典と根拠

ORDレコード
ord-e1f4ed265e034a7a8b4bb2f32b32ba0d
出典データセット
uspto-grants-2010_05
特許番号
US07709503B2

反応ノート

読み込み中…