Acetyl chloride → N-((2-chloro-4-morpholinothieno[3,2-d]pyrimidin-6-yl)methyl)-N-methylacetamide

HRID 2098700ノート

反応式

HRID 2098700 の反応式
[Cl:1][C:2]1[N:3]=[C:4]([N:14]2[CH2:19][CH2:18][O:17][CH2:16][CH2:15]2)[C:5]2[S:10][C:9]([CH2:11][NH:12][CH3:13])=[CH:8][C:6]=2[N:7]=1.[C:20](Cl)(=[O:22])[CH3:21].C(N(CC)CC)C>ClCCl>[Cl:1][C:2]1[N:3]=[C:4]([N:14]2[CH2:19][CH2:18][O:17][CH2:16][CH2:15]2)[C:5]2[S:10][C:9]([CH2:11][N:12]([CH3:13])[C:20](=[O:22])[CH3:21])=[CH:8][C:6]=2[N:7]=1

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 595929371-(2-Chloro-4-morpholinothieno[3,2-d]pyrimidin-6-yl)-N-methylmethanamine

生成物 1

HCID 59829246N-((2-chloro-4-morpholinothieno[3,2-d]pyrimidin-6-yl)methyl)-N-methylacetamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of (2-Chloro-4-morpholin-4-yl-thieno[3,2-d]pyrimidin-6-ylmethyl)-methylamine (120 mg) in dichloromethane (2 ml) was added acetyl chloride (31.4 μL) and triethylamine (61.6 μL). The reaction mixture was stirred at room temperature for 3.5 hours, then diluted with dichloromethane, washed with brine, dried (MgSO4) and the solvents removed in vacuo to give a crude residue. This was purified by flash chromatography to yield N-(2-Chloro-4-morpholin-4-yl-thieno[3,2-d]pyrimidin-6-ylmethyl)-N-methyl-acetamide (110 mg).

後処理

  1. washwashed with brine
  2. dry with materialdried (MgSO4)
  3. customthe solvents removed in vacuo
  4. customto give a crude residue
  5. customThis was purified by flash chromatography

出典と根拠

ORDレコード
ord-4ad48eb07f4549acacf3c80a190508b7
出典データセット
uspto-grants-2013_05
特許番号
US08450315B2

反応ノート

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