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Methylamine → HCID 178485847、化合物

HRID 1408424
ノート
印刷プレビュー

反応式

HRID 1408424 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:12]=[CH:11][NH:10][N:9]=2)=[CH:4][C:3]=1[CH2:13][NH2:14].C([C:22]1[NH:23][CH:24]=CN=1)(C1NC=CN=1)=O.CN.C1C[O:32]CC1>ClCCl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:12]=[CH:11][NH:10][N:9]=2)=[CH:4][C:3]=1[CH2:13][NH:14][C:24]([NH:23][CH3:22])=[O:32]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6329MethylamineHCID 8028Tetrahydrofuran2 回HCID 5250894Bis-(1H-imidazol-2-YL)-methanoneHCID 178509482HCID 178509482、化合物

生成物 1

HCID 178485847HCID 178485847、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 2-chloro-5-(1H-pyrazol-3-yl)benzenemethanamine (i.e. the product of Step C of Synthesis Example 4) (2.4 g, 11.6 mmol) in THF (12 mL) and dichloromethane (12 mL) at 10° C. was added carbonyl diimidazole (2.8 g, 17.3 mmol). The reaction mixture was stirred at ambient temperature for 30 minutes and then cooled to 0° C. A solution of methylamine in THF (2 M, 12.0 mL, 24 mmol) was added, and the reaction mixture was stirred at ambient temperature for 15 h. The reaction mixture was then diluted with dichloromethane, washed with water and brine, concentrated and purified by preparative TLC (2% methanol in chloroform as eluant) to provide the title product as a solid (1.0 g).

後処理

  1. temperaturecooled to 0° C
  2. stirringthe reaction mixture was stirred at ambient temperature for 15 h
  3. washwashed with water and brine
  4. concentrationconcentrated
  5. custompurified by preparative TLC (2% methanol in chloroform as eluant)

出典と根拠

ORDレコード
ord-1e2a5676f5774b93b10c40b6f9f39898
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08921360B2

反応ノート

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