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Triethylamine → N-[(2-amino-1,3-thiazol-4-yl)methyl]-6-chloro-5-fluoro-2-methyl-4-pyrimidinamine

HRID 1366489
ノート
印刷プレビュー

反応式

HRID 1366489 の反応式
Cl[C:2]1[C:7]([F:8])=[C:6]([Cl:9])[N:5]=[C:4]([CH3:10])[N:3]=1.C[NH:12][CH2:13][C:14]1[N:15]=[C:16]([NH2:19])[S:17][CH:18]=1.C(N(CC)CC)C>C1COCC1>[NH2:19][C:16]1[S:17][CH:18]=[C:14]([CH2:13][NH:12][C:2]2[C:7]([F:8])=[C:6]([Cl:9])[N:5]=[C:4]([CH3:10])[N:3]=2)[N:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 137310334,6-Dichloro-5-fluoro-2-methylpyrimidineHCID 189398714-((Methylamino)methyl)thiazol-2-amine

生成物 1

HCID 86636959N-[(2-amino-1,3-thiazol-4-yl)methyl]-6-chloro-5-fluoro-2-methyl-4-pyrimidinamine収率 62%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4,6-Dichloro-5-fluoro-2-methylpyrimidine (480 mg, 2.65 mmol) was dissolved in 20 mL of THF and stirred at room temperature. (4-[(Methylamino)methyl]-1,3-thiazol-2-amine (2.65 mmol, theoretical) was added, followed by triethylamine (400 μL, 2.92 mmol). The resulting reaction mixture was stirred overnight and evaporated. The residue was stirred in water and the solid precipitate was collected by filtration and was dried in vacuo to provide N-[(2-amino-1,3-thiazol-4-yl)methyl]-6-chloro-5-fluoro-2-methyl-4-pyrimidinamine (450 mg, 59%) that was used without further purification. LCMS: (M+H)+: 288.1.

後処理

  1. customThe resulting reaction mixture
  2. stirringwas stirred overnight
  3. customevaporated
  4. stirringThe residue was stirred in water
  5. filtrationthe solid precipitate was collected by filtration
  6. customwas dried in vacuo

出典と根拠

ORDレコード
ord-e64767c8fdea4014a0fc9455e508827b
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07893056B2

反応ノート

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