2-Bromo-1,3-thiazole-5-carbonitrile → HCID 68580052, 화합물

HRID 2234049노트

반응식

HRID 2234049 반응식
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]

참가 물질

5

반응물 2

HCID 178609522-Bromo-1,3-thiazole-5-carbonitrileHCID 68579996HCID 68579996, 화합물2회

생성물 1

HCID 68580052HCID 68580052, 화합물

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6a987e3030e84b81a1ff67f8793c1b32
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709503B2

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