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Water → 6-Chloro-N-(2-pyridinylmethyl)-4-pyrimidinamine

HRID 58164
ノート
印刷プレビュー

反応式

HRID 58164 の反応式
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[CH:4][N:3]=1.CCN(C(C)C)C(C)C.[N:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[CH2:24][NH2:25].O>CC(O)C>[Cl:8][C:6]1[N:5]=[CH:4][N:3]=[C:2]([NH:25][CH2:24][C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][N:18]=2)[CH:7]=1
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 962WaterHCID 195092-PyridinemethanamineHCID 709434,6-DichloropyrimidineHCID 81531Diisopropylethylamine

生成物 1

HCID 534102726-Chloro-N-(2-pyridinylmethyl)-4-pyrimidinamine収率 78%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

このページの内容参加物実験手順後処理出典と根拠反応ノート

To a solution of 4,6-dichloro-pyrimidine (1 g, 7 mmol) in iPrOH (40 mL) and DIPEA (1.16 g, 9 mmol) was added a solution of 2-pyridinylmethanamine (970 g, 9 mmol) at room temperature. The resulting mixture was stirred at room temperature for 2.5 hours. Water was added and the mixture was extracted with DCM. The combined extracts were washed with brine, dried over anhydrous sodium sulfate and concentrated to give a crude product, which was purified by flash chromatography on silica to obtain the title compound (1.2 g, yield: 78%). MS (ESI): 221 [M+H]+.

後処理

  1. extractionthe mixture was extracted with DCM
  2. washThe combined extracts were washed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. customto give a crude product, which
  6. customwas purified by flash chromatography on silica

出典と根拠

ORDレコード
ord-fc5e87935fb649a98361c1c74cfdadd2
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09434697B2

反応ノート

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