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Methylamine → 1-Methyl-3-(4-methyl-5-pyridin-4-yl-thiazol-2-yl)-urea

HRID 1951185
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반응식

HRID 1951185 반응식
CN.[CH3:3][C:4]1[N:5]=[C:6]([NH:15][C:16]([N:18]2C=CN=[CH:19]2)=[O:17])[S:7][C:8]=1[C:9]1[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=1>O.CN(C=O)C>[CH3:19][NH:18][C:16]([NH:15][C:6]1[S:7][C:8]([C:9]2[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=2)=[C:4]([CH3:3])[N:5]=1)=[O:17]
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참가 물질

5

반응물 2

HCID 6329MethylamineHCID 86610330Imidazole-1-carboxylic acid (4-methyl-5-pyridin-4-yl-thiazol-2-yl)-amide

생성물 1

HCID 866103291-Methyl-3-(4-methyl-5-pyridin-4-yl-thiazol-2-yl)-urea

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

Methylamine (0.030 ml of a 40% w/w/solution in water, 0.351 mmol) is added to a stirred suspension of imidazole-1-carboxylic acid (4-methyl-5-pyridin-4-yl-thiazol-2-yl)-amide (18a) (0.1 g, 0.351 mmol) in DMF (3 ml). The reaction mixture is stirred at room temperature for 1 hour and then the solvent is removed in vacuo. The crude product is dissolved in THF/DMF (10:1, 3 ml) and passed through a polymer supported isocyanate resin (0.9 g, 1.1 mmol/g loading) and washed through with THF. The solution is concentrated in vacuo and the residue washed with ethyl acetate and methanol to afford the titled compound.

후처리

  1. customthe solvent is removed in vacuo
  2. dissolutionThe crude product is dissolved in THF/DMF (10:1, 3 ml)
  3. washwashed through with THF
  4. concentrationThe solution is concentrated in vacuo
  5. washthe residue washed with ethyl acetate and methanol

출처 및 근거

ORD 기록
ord-332930a20f4148038676fee0335c1329
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08404684B2

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