Triethylamine → 2-{[2-(Methanesulfonylamino)ethyl]amino}-4-(3-methylanilino)pyrimidine-5-carboxamide

HRID 2303309ノート

反応式

HRID 2303309 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].C(N(CC)CC)C.[NH2:13][CH2:14][CH2:15][NH:16][C:17]1[N:22]=[C:21]([NH:23][C:24]2[CH:29]=[CH:28][CH:27]=[C:26]([CH3:30])[CH:25]=2)[C:20]([C:31]([NH2:33])=[O:32])=[CH:19][N:18]=1>C(OCC)(=O)C>[CH3:1][S:2]([NH:13][CH2:14][CH2:15][NH:16][C:17]1[N:22]=[C:21]([NH:23][C:24]2[CH:29]=[CH:28][CH:27]=[C:26]([CH3:30])[CH:25]=2)[C:20]([C:31]([NH2:33])=[O:32])=[CH:19][N:18]=1)(=[O:4])=[O:3]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 98173492-(2-Aminoethylamino)-4-(m-tolylamino)pyrimidine-5-carboxamide

生成物 1

HCID 184608482-{[2-(Methanesulfonylamino)ethyl]amino}-4-(3-methylanilino)pyrimidine-5-carboxamide

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A 114 μl portion of methanesulfonyl chloride and 205 μl of triethylamine were added to a mixture of 382 mg of 2-(2-aminoethylamino)-4-(3-methylanilino)pyrimidine-5-carboxamide with 10 ml of ethyl acetate, followed by stirring at room temperature for 3.5 hours. The reaction mixture was washed with water and saturated brine, and then the organic layer was dried over anhydrous magnesium sulfate. This was concentrated under a reduced pressure and the resulting residue was recrystallized from a mixed solvent of methanol and ethyl acetate to obtain 210 mg of 2-{[2-(methanesulfonylamino)ethyl]amino}-4-(3-methylanilino)pyrimidine-5-carboxamide (colorless crystals).

後処理

  1. washThe reaction mixture was washed with water and saturated brine
  2. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  3. concentrationThis was concentrated under a reduced pressure
  4. customthe resulting residue was recrystallized from a mixed solvent of methanol and ethyl acetate

出典と根拠

ORDレコード
ord-c1d78e4fc76549d98b5f58066eee71dc
出典データセット
uspto-grants-2002_08
特許番号
US06432963B1

反応ノート

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