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Dichloromethane → 2-(4-(6-Chloro-2-methylpyrimidin-4-yl)piperazin-1-yl)ethanol

HRID 515245
ノート
印刷プレビュー

反応式

HRID 515245 の反応式
[OH:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.[CH3:10][C:11]1[N:16]=[C:15](Cl)[CH:14]=[C:13]([Cl:18])[N:12]=1.C(Cl)Cl>C(N(CC)CC)C>[Cl:18][C:13]1[N:12]=[C:11]([CH3:10])[N:16]=[C:15]([N:7]2[CH2:8][CH2:9][N:4]([CH2:3][CH2:2][OH:1])[CH2:5][CH2:6]2)[CH:14]=1
参加物反応条件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 6344DichloromethaneHCID 76771-(2-Hydroxyethyl)piperazine2 回HCID 2349974,6-Dichloro-2-methylpyrimidine2 回

生成物 1

HCID 144795582-(4-(6-Chloro-2-methylpyrimidin-4-yl)piperazin-1-yl)ethanol収率 89.8%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

反応条件

温度
30 °C

実験手順

1-(2-hydroxyethyl)piperazine (Compound 3) (16.6 g, 127.6 mmol)) and 2-methyl-4,6-dichloropyrimidine (Compound 2) (10.4 g, 63.8 mmol) were mixed with methylene dichloride (80 mL) in reaction flask to be stirred for 2.5 h at 30° C., and then triethylamine (1.8 mL) was added with the reaction overnight in thermal insulation. After vacuum filtration, the cake was rinsed by methylene dichloride. The filtrate was vacuum condensed to dry, and then n-hexane (40 mL) was added to grow the grains for 1 h by stirring. After vacuum filtration, the cake was rinsed by n-hexane (20 mL) and dried at 40° C. to constant weight to give white solid target Compound 4 (14.7 g, yield: 89.8%).

後処理

  1. filtrationAfter vacuum filtration
  2. washthe cake was rinsed by methylene dichloride
  3. customvacuum condensed
  4. customto dry
  5. additionn-hexane (40 mL) was added
  6. customfor 1 h
  7. stirringby stirring
  8. filtrationAfter vacuum filtration
  9. washthe cake was rinsed by n-hexane (20 mL)
  10. customdried at 40° C. to constant weight

出典と根拠

ORDレコード
ord-9c2895924dc74897ab2ed8b4c70ac49f
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09108954B2

反応ノート

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