3-Amino-1-propanol → HCID 135433506、化合物

HRID 363364ノート

反応式

HRID 363364 の反応式
Cl[C:2]1[CH:7]=[C:6]([OH:8])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[O:15][CH2:16][CH2:17][CH3:18])[N:3]=1.[NH2:19][CH2:20][CH2:21][CH2:22][OH:23]>C(O)CC>[OH:23][CH2:22][CH2:21][CH2:20][NH:19][C:2]1[N:3]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[O:15][CH2:16][CH2:17][CH3:18])[NH:5][C:6](=[O:8])[CH:7]=1

参加物

4

反応物 2

HCID 90863-Amino-1-propanolHCID 178458304HCID 178458304、化合物

生成物 1

HCID 135433506HCID 135433506、化合物

試薬・触媒・溶媒 1

HCID 10311-Propanol溶媒

実験手順

A stirred solution of 4-chloro-6-hydroxy-2-(2-propoxyphenyl)pyrimidine (0.66 g) and 3-amino-1-propanol (0.56 g) in n-propanol was heated under reflux for 16 hours. The cooled reaction mixture was evaporated under reduced pressure to yield an oil which was partitioned between chloroform (20 ml) and water (20 ml). The chloroform layer was separated from the aqueous layer which was extracted with chloroform (2×10 ml) and the combined chloroform layers were washed with water, dried (magnesium sulfate) and evaporated under reduced pressure. The residue was recrystallized from isopropanol:diethyl ether to yield the title compound, 0.54 g, m.p. 147.5°-148.5° C.

後処理

  1. temperatureunder reflux for 16 hours
  2. customThe cooled reaction mixture
  3. customwas evaporated under reduced pressure
  4. customto yield an oil which
  5. customwas partitioned between chloroform (20 ml) and water (20 ml)
  6. customThe chloroform layer was separated from the aqueous layer which
  7. extractionwas extracted with chloroform (2×10 ml)
  8. washthe combined chloroform layers were washed with water
  9. dry with materialdried (magnesium sulfate)
  10. customevaporated under reduced pressure
  11. customThe residue was recrystallized from isopropanol

出典と根拠

ORDレコード
ord-01a017a6fdcc498cab036fb016f8a4dd
出典データセット
uspto-grants-1999_02
特許番号
US05874440

反応ノート

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