Acetone → 2-Chloro-4,6-bis(morpholin-4-yl)-1,3,5-triazine

HRID 404404

反応式

HRID 404404 の反応式
[N:1]1[C:8](Cl)=[N:7][C:5](Cl)=[N:4][C:2]=1[Cl:3].C([N:12]([CH2:15][CH3:16])[CH2:13][CH3:14])C.[NH:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1.CC(C)=[O:25]>O>[Cl:3][C:2]1[N:1]=[C:8]([N:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)[N:7]=[C:5]([N:12]2[CH2:13][CH2:14][O:25][CH2:16][CH2:15]2)[N:4]=1

参加物

6

反応物 4

HCID 180AcetoneHCID 7954Cyanuric chlorideHCID 8083MorpholineHCID 8471Triethylamine

生成物 1

HCID 2249672-Chloro-4,6-bis(morpholin-4-yl)-1,3,5-triazine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a stirred solution of cyanuric chloride (18.4 g, 10 mmol) in acetone (100 ml) and crushed ice (500 g), a mixture of triethylamine (30.0 g, excess) and morpholine (17.4 g, 20 mmol) was added at −10° C. After the addition, reaction mixture was stirred at room temperature and for 1 hour and diluted with 50 ml water. Separated white solid was filtered and washed with water. The white solid was dried and filtered. The crude product was found to be pure and taken to next step without purification. Yield: 25 g, 87%; (M+H) 286.7

後処理

  1. additionwas added at −10° C
  2. additionAfter the addition, reaction mixture
  3. customSeparated white solid
  4. filtrationwas filtered
  5. washwashed with water
  6. customThe white solid was dried
  7. filtrationfiltered
  8. customtaken to next step without purification

出典と根拠

ORDレコード
ord-34c660371fc240228bac8fd8cf0e334a
出典データセット
uspto-grants-2014_06
特許番号
US08748421B2

関連ノート

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