Isopropylamine → 4-(Isopropylamino)-1-(o-methoxyphenoxy)-2-butanol Hydrochloride

HRID 485947ノート

反応式

HRID 485947 の反応式
[CH3:1][O:2][C:3]1[CH:15]=[CH:14][CH:13]=[CH:12][C:4]=1[O:5][CH:6]([Cl:11])[CH:7]([OH:10])[CH2:8][CH3:9].[CH:16]([NH2:19])([CH3:18])[CH3:17]>C(O)CCC>[ClH:11].[CH:16]([NH:19][CH2:9][CH2:8][CH:7]([OH:10])[CH2:6][O:5][C:4]1[CH:12]=[CH:13][CH:14]=[CH:15][C:3]=1[O:2][CH3:1])([CH3:18])[CH3:17]

参加物

4

反応物 2

HCID 6363IsopropylamineHCID 198402361-(2-Methoxyphenoxy)-2-hydroxybutyl chloride

生成物 1

HCID 131203654-(Isopropylamino)-1-(o-methoxyphenoxy)-2-butanol Hydrochloride

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
120 °C

実験手順

A mixture which contained 11.6 g. (0.05 mole) of 1-(2-methoxyphenoxy)-2-hydroxybutyl chloride, 50 ml. of isopropyl amine and 100 ml. of n-butanol was charged in a steel bomb and heated at 120° C. for 24 hr. The resulting reaction mixture was filtered. The filtrate was concentrated to dryness and mixed with 200 ml. of 3N hydrochloric acid, extracted with ether and the aqueous layer was made basic. The base insoluble oil was extracted into isopropyl ether, dried over sodium sulfate and concentrated to dryness. The residue was dissolved in isopropanol and mixed with 20 ml. ethereal hydrogen chloride. The gummy precipitate recrystallized using isopropyl ether and isopropanol. The hydrochloride (8.3 g.) melted at 83°-85° C.

後処理

  1. customThe resulting reaction mixture
  2. filtrationwas filtered
  3. concentrationThe filtrate was concentrated to dryness
  4. additionmixed with 200 ml
  5. extractionof 3N hydrochloric acid, extracted with ether
  6. extractionThe base insoluble oil was extracted into isopropyl ether
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated to dryness
  9. dissolutionThe residue was dissolved in isopropanol
  10. additionmixed with 20 ml
  11. customThe gummy precipitate recrystallized

出典と根拠

ORDレコード
ord-022ea6a616814bafb51827c38554d339
出典データセット
uspto-grants-1985_08
特許番号
US04538001

反応ノート

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