Ammonium Chloride → HCID 178433654, 화합물

HRID 2234006노트

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HRID 2234006 반응식
[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]

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 68580052HCID 68580052, 화합물

생성물 1

HCID 178433654HCID 178433654, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
120 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-e1f4ed265e034a7a8b4bb2f32b32ba0d
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709503B2

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