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

HRID 64700노트

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HRID 64700 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 2631-Butanol용매

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온도
120 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-737c20bec0cd4c9abc4238a88eeccc81
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04609735

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