Cesium carbonate → 5-(4-iodo-2-methyl-imidazol-1-yl)-2-methyl-2H-pyridazin-3-one

HRID 2194415

반응식

HRID 2194415 반응식
Cl[C:2]1[CH:7]=[N:6][N:5]([CH3:8])[C:4](=[O:9])[CH:3]=1.[I:10][C:11]1[N:12]=[C:13]([CH3:16])[NH:14][CH:15]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C>[I:10][C:11]1[N:12]=[C:13]([CH3:16])[N:14]([C:2]2[CH:7]=[N:6][N:5]([CH3:8])[C:4](=[O:9])[CH:3]=2)[CH:15]=1

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 129101445-Chloro-2-methylpyridazin-3(2H)-oneHCID 178433060HCID 178433060, 화합물

생성물 1

HCID 668656855-(4-iodo-2-methyl-imidazol-1-yl)-2-methyl-2H-pyridazin-3-one수율 71.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
45 °C

실험 절차

To a solution of 160 mg (1.11 mmol) of 5-chloro-2-methyl-2H-pyridazin-3-one (CAS: [14628-34-3]), 230 mg (1.11 mmol) of 4-iodo-2-methyl-1H-imidazole (CAS: [73746-45-9]), in 3.5 ml of dry DMF were added 721 mg (2.21 mmol) of cesium carbonate. The suspension was stirred for 30 min at 45° C., then for 3 h at 65° C. and allowed to cool. The cristallised product is filtered off, washed with ethyl acetate and dried in vaccuo to yield 250 mg (0.791 mmol, 71%) of the title compound as a crystalline light yellow solid, MS: m/e=316.9 (M+H+).

후처리

  1. waitfor 3 h at 65° C.
  2. temperatureto cool
  3. filtrationThe cristallised product is filtered off
  4. washwashed with ethyl acetate
  5. customdried in vaccuo

출처 및 근거

ORD 기록
ord-fb33a895c6bf45c08330c5a5f7d30a76
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08334287B2

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