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

HRID 638713

反応式

HRID 638713 の反応式
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

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 66811347HCID 66811347、化合物

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-32f92b863a8d4b1fb2cc60978d75aa91
出典データセット
uspto-grants-2010_04
特許番号
US07691364B2

関連ノート

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