Triethylamine → HCID 23435529、化合物

HRID 860078

反応式

HRID 860078 の反応式
Cl[C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[C:4]([Cl:9])[N:3]=1.Cl.[CH2:11]([NH2:13])[CH3:12].CCN(CC)CC>C(O)CCC>[NH2:8][C:6]1[CH:5]=[C:4]([Cl:9])[N:3]=[C:2]([NH:13][CH2:11][CH3:12])[N:7]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 11198Ethylamine hydrochlorideHCID 823874-Pyrimidinamine, 2,6-dichloro-

生成物 1

HCID 23435529HCID 23435529、化合物

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
90 °C

実験手順

A mixture of 2,6-dichloro-4-aminopyrimidine 18-1 (Avocado; 4.8 g, 29.3 mmol), ethylamine hydrochloride (7.0 g, 85.8 mmol), Et3N (20 mL, 144 mmol) and n-butanol (150 mL) was heated to 90° C. for 6 hours. After cooling, the solvent was removed in vacuo and the residue partitioned between saturated Na2CO3 solution and EtOAc. The EtOAc layer was washed with brine, dried (MgSO4) and concentrated to give an orange solid. Purification by column chromatography (EtOAc/hexane 1:1) gave the title compound 18-2 as a white solid.

後処理

  1. temperatureAfter cooling
  2. customthe solvent was removed in vacuo
  3. customthe residue partitioned between saturated Na2CO3 solution and EtOAc
  4. washThe EtOAc layer was washed with brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customto give an orange solid
  8. customPurification by column chromatography (EtOAc/hexane 1:1)

出典と根拠

ORDレコード
ord-f375066a496849a29a18fbc735d95bb3
出典データセット
uspto-grants-2006_12
特許番号
US07153862B2

関連ノート

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