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Methylamine → 3-Diphenylmethoxy-1-methylazetidine

HRID 654081
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HRID 654081 반응식
Cl[CH2:2][CH:3]([O:6][CH:7]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[CH2:4]Cl.[CH3:20][NH2:21]>>[C:8]1([CH:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[O:6][CH:3]2[CH2:4][N:21]([CH3:20])[CH2:2]2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 6329MethylamineHCID 123293381,3-Dichloro-2-diphenylmethoxypropane

생성물 1

HCID 198883633-Diphenylmethoxy-1-methylazetidine

실험 절차

A solution of 244. g (0.83 mole) of 1,3-dichloro-2-diphenylmethoxypropane in 300 ml of methylamine was heated in a steel bomb to 100° for 18 hours. The mixture was concentrated, and the residue partitioned between chloroform and dilute hydrochloric acid. The acid solution was washed twice with chloroform, and the chloroform solutions combined. The chloroform was extracted with dilute sodium hydroxide, dried with sodium sulfate, and concentrated. The residue was distilled (b.p. 125°-130°/0.1 mm) to yield 104 g (40%). The distillate crystallizes on standing and can be recrystallized from isooctane, mp 44°-48°.

후처리

  1. concentrationThe mixture was concentrated
  2. customthe residue partitioned between chloroform and dilute hydrochloric acid
  3. washThe acid solution was washed twice with chloroform
  • extractionThe chloroform was extracted with dilute sodium hydroxide
  • dry with materialdried with sodium sulfate
  • concentrationconcentrated
  • distillationThe residue was distilled (b.p. 125°-130°/0.1 mm)
  • customto yield 104 g (40%)
  • customThe distillate crystallizes on standing
  • customcan be recrystallized from isooctane, mp 44°-48°
  • 출처 및 근거

    ORD 기록
    ord-bd305e8849c54c68bf5833864a402d91
    출처 데이터셋
    uspto-grants-1992_07
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05130309

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