Hydrochloric Acid → 6-(4-Aminophenoxy)-hexanoic acid methyl ester

HRID 638713

반응식

HRID 638713 반응식
Cl.[NH2:2][C:3]1[CH:17]=[CH:16][C:6]([O:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([OH:15])=[O:14])=[CH:5][CH:4]=1.Cl.[CH3:19]O>>[CH3:19][O:14][C:13](=[O:15])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][O:7][C:6]1[CH:5]=[CH:4][C:3]([NH2:2])=[CH:17][CH:16]=1

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 66811347HCID 66811347, 화합물

생성물 1

HCID 146502966-(4-Aminophenoxy)-hexanoic acid methyl ester

실험 절차

To a mixture of 6-(4-Amino-phenoxy)-hexanoic acid hydrochloride 20 (150 grams, 578 mmol) in methanol (3 liters) was passed dry HCl gas at 10° C. for 1 hour and refluxed for 48 hours. Methanol (1.5 liter) was distilled off, ice water (1 liter) was added and the pH was adjusted to 7.5 with K2CO3. Crude 21 was extracted into chloroform, washed with 5% NaHCO3 solution in water, dried over Na2SO4 and distilled to give 21 (60 g, 43.8) as a thick brown syrup. The structure was confirmed with NMR.

후처리

  1. customat 10° C.
  2. customfor 1 hour
  3. temperaturerefluxed for 48 hours
  4. distillationMethanol (1.5 liter) was distilled off
  5. additionice water (1 liter) was added
  6. extractionCrude 21 was extracted into chloroform
  7. washwashed with 5% NaHCO3 solution in water
  8. dry with materialdried over Na2SO4
  9. distillationdistilled

출처 및 근거

ORD 기록
ord-32f92b863a8d4b1fb2cc60978d75aa91
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07691364B2

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