Hydrogen Bromide → gamma-Morpholinobutyric acid hydrobromide

HRID 2071977노트

반응식

HRID 2071977 반응식
[O:1]1[CH2:6][CH2:5][N:4]([CH2:7][CH2:8][CH2:9][C:10]([O:12]C)=[O:11])[CH2:3][CH2:2]1.[BrH:14]>O>[BrH:14].[O:1]1[CH2:2][CH2:3][N:4]([CH2:7][CH2:8][CH2:9][C:10]([OH:12])=[O:11])[CH2:5][CH2:6]1

참가 물질

4

실험 절차

15 g. (0.052 mole) of methyl γ-morpholinobutyrate [Cruickshank and Sheehan, J. Am. Chem. Soc. 83 2891 (1961)] was dissolved in a mixture of 45 ml. of 47% hydrobromic acid and 45 ml. of water and heated for 16 hours at reflux. The solution was taken to dryness under reduced pressure, and the solid which formed was triturated with acetone. The material was filtered and crystallized from 60 ml. of acetic acid to give 12.4 g. (95%) of product as colorless crystals, m.p. 151° - 152.5°. The infrared and nmr spectra are consistent with the proposed structure.

후처리

  1. temperatureat reflux
  2. customthe solid which formed
  3. customwas triturated with acetone
  4. filtrationThe material was filtered
  5. customcrystallized from 60 ml
  6. customof acetic acid to give 12.4 g

출처 및 근거

ORD 기록
ord-997c5258628740bfbc1e7d926bf43842
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04049653

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