Triethylamine → HCID 178451230, 화합물

HRID 1620608노트

반응식

HRID 1620608 반응식
Cl.[NH2:2][CH2:3][C:4]([O:6][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:5].C(N(CC)CC)C.S=[C:19]1[CH2:23][S:22][C:21](=[O:24])[NH:20]1>C(O)C>[O:24]=[C:21]1[N:20]=[C:19]([NH:2][CH2:3][C:4]([O:6][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:5])[CH2:23][S:22]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 15395954-Sulfanylidene-1,3-thiazolidin-2-oneHCID 2725036Glycine tert-butyl ester hydrochloride

생성물 1

HCID 178451230HCID 178451230, 화합물수율 58.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of tert-butyl glycinate hydrochloride (4.00 g) and triethylamine (3.33 mL) in ethanol (20 mL) was added 4-thioxo-1,3-thiazolidin-2-one (2.65 g), and the mixture was stirred at room temperature for 4 hr. The reaction mixture was concentrated under reduced pressure, water was added to the residue, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (2.70 g).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure, water
  2. additionwas added to the residue
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-1f2969ed58cb4406b3f9155ce378264e
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772277B2

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