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Hydrochloric Acid → 2-[4-[3-(Benzyloxy)-3-oxopropyl]-8-(3-methylbutylidene)-3-oxo-1-thia-4-azaspiro[4.5]decan-2-yl]-acetic acid

HRID 1934734
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인쇄 미리보기

반응식

HRID 1934734 반응식
[CH3:1][CH:2]([CH3:12])[CH2:3][CH:4]=[C:5]1[CH2:10][CH2:9][C:8](=O)[CH2:7][CH2:6]1.[NH2:13][CH2:14][CH2:15][C:16]([O:18][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[O:17].[SH:26][CH:27]([CH2:31][C:32]([OH:34])=[O:33])[C:28](O)=[O:29].Cl>C(OCC)(=O)C.C1(C)C=CC=CC=1>[CH2:19]([O:18][C:16](=[O:17])[CH2:15][CH2:14][N:13]1[C:8]2([CH2:9][CH2:10][C:5](=[CH:4][CH2:3][CH:2]([CH3:12])[CH3:1])[CH2:6][CH2:7]2)[S:26][CH:27]([CH2:31][C:32]([OH:34])=[O:33])[C:28]1=[O:29])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1
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참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6268(+-)-Mercaptosuccinic acidHCID 1116164Benzyl 3-aminopropanoateHCID 11636865HCID 11636865, 화합물

생성물 1

HCID 224671502-[4-[3-(Benzyloxy)-3-oxopropyl]-8-(3-methylbutylidene)-3-oxo-1-thia-4-azaspiro[4.5]decan-2-yl]-acetic acid수율 59%

시약·촉매·용매 2

HCID 1140
Toluene
용매
HCID 8857Ethyl Acetate용매

실험 절차

To 20 ml of toluene were added 1.90 g of 4-(3-methylbutylidene)-1-cyclohexanone and 2.05 g of benzyl 3-aminopropionate, and the mixture was stirred at ambient temperature for one hour. Then, 1.72 g of mercaptosuccinic acid was added, and the resulting mixture was heated under reflux for one hour under the condition of azeotropic dehydration by means of Dean Stark. The reaction mixture was added to a mixture of ice water and ethyl acetate, pH was adjusted to 2.0 with 2 mol/L hydrochloric acid, and the organic layer was separated. The organic layer was washed successively with water and saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue thus obtained was purified by column chromatography [eluent: chloroform:ethanol=50:1] to obtain 3.10 g of 2-[4-[3-(benzyloxy)-3-oxopropyl]-8-(3-methylbutylidene)-3-oxo-1-thia-4-azaspiro[4.5]decan-2-yl]-acetic acid as a light yellow oily product.

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for one hour under the condition of azeotropic dehydration by means of Dean Stark
  3. customthe organic layer was separated
  4. washThe organic layer was washed successively with water and saturated aqueous solution of sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue thus obtained
  8. customwas purified by column chromatography [eluent: chloroform:ethanol=50:1]

출처 및 근거

ORD 기록
ord-ce5c135664fd48cd88f2b7452942bd5b
출처 데이터셋
uspto-grants-2002_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06384065B1

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