Water → (3,6-Dichloropyridazin-4-yl)diethylamine

HRID 217704

反応式

HRID 217704 の反応式
[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1Cl.[CH2:10]([NH:12][CH2:13][CH3:14])[CH3:11].O.CC(=O)OCC>C1(C)C=CC=CC=1>[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[N:12]([CH2:13][CH3:14])[CH2:10][CH3:11]

参加物

6

反応物 4

HCID 962WaterHCID 8021DiethylamineHCID 8857Ethyl AcetateHCID 951233,4,6-Trichloropyridazine

生成物 1

HCID 58136930(3,6-Dichloropyridazin-4-yl)diethylamine

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

3,4,6-Trichloropyridazine (2 g) and diethylamine (2.4 ml) were initially charged in toluene (10 ml) and left to stand at RT for 3 days. Then the mixture was admixed with water and EA, and the EA phase was removed. The EA phase was washed three times with water, dried over magnesium sulfate, filtered and concentrated. The residue was purified using silica gel (70 g cartridge, n-heptane/EA gradient 0-50% within 60 min). 1.1 g of the title compound were obtained.

後処理

  1. waitleft
  2. customthe EA phase was removed
  3. washThe EA phase was washed three times with water
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified
  8. customsilica gel (70 g cartridge, n-heptane/EA gradient 0-50% within 60 min)

出典と根拠

ORDレコード
ord-8b427b2e1e5a481394b1b715a71e768f
出典データセット
uspto-grants-2012_06
特許番号
US08198272B2

関連ノート

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