2-Bromo-1,3-thiazole-5-carbonitrile → HCID 68580052、化合物

HRID 2234049ノート

反応式

HRID 2234049 の反応式
Cl.[Cl:2][C:3]1[C:7]([Cl:8])=[C:6]([CH3:9])[NH:5][C:4]=1[C:10]([NH:12][CH:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1)=[O:11].Br[C:20]1[S:21][C:22]([C:25]#[N:26])=[CH:23][N:24]=1>CN1C(=O)CCC1.CCOC(C)=O>[Cl:2][C:3]1[C:7]([Cl:8])=[C:6]([CH3:9])[NH:5][C:4]=1[C:10]([NH:12][CH:13]1[CH2:18][CH2:17][N:16]([C:20]2[S:21][C:22]([C:25]#[N:26])=[CH:23][N:24]=2)[CH2:15][CH2:14]1)=[O:11]

参加物

5

反応物 2

HCID 178609522-Bromo-1,3-thiazole-5-carbonitrileHCID 68579996HCID 68579996、化合物2 回

生成物 1

HCID 68580052HCID 68580052、化合物

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

To a solution of 3,4-dichloro-5-methyl-N-piperidin-4-yl-1H-pyrrole-2-carboxamide hydrochloride (Intermediate 1; 0.330 g, 1.058 mmol) in NMP (2 ml) was added TEA (0.150 ml, 1.058 mmol) followed by the addition of 2-bromo-1,3-thiazole-5-carbonitrile (prepared according to F. Campagna et al. Tet. Lett, 1977, 21, 1815-1816) (0.200 g, 1.058 mmol) at room temperature. Using a Smith Microwave Synthesizer, the mixture was subjected to single-mode microwave at 150° C. for 20 minutes. The crude mixture was diluted with EtOAc and washed with water several times. The extracts were combined dried over magnesium sulfate and concentrated to give the desired product. (0.450 g).

後処理

  1. customat 150° C.
  2. customfor 20 minutes
  3. washwashed with water several times
  4. dry with materialThe extracts were combined dried over magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-6a987e3030e84b81a1ff67f8793c1b32
出典データセット
uspto-grants-2010_05
特許番号
US07709503B2

反応ノート

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