Hydrogen Bromide → gamma-Morpholinobutyric acid hydrobromide

HRID 267339노트

반응식

HRID 267339 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

반응물 2

HCID 260Hydrogen BromideHCID 44858Methyl 4-morpholinobutanoate

생성물 1

HCID 68121683gamma-Morpholinobutyric acid hydrobromide

시약·촉매·용매 1

HCID 962Water용매

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°C. The infrared and nuclear magnetic resonance spectra were 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-b6f5b4f513de4a1696a4503087708966
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03941782

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