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Ethyl Acetate → 2-(Benzylthio)-3-thiomorpholinopropan-1-amine

HRID 504803
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인쇄 미리보기

반응식

HRID 504803 반응식
[CH2:1]([S:8][CH:9]([CH2:19][N:20]1[CH2:25][CH2:24][S:23][CH2:22][CH2:21]1)[CH2:10][NH:11]C(=O)OC(C)(C)C)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(OCC)(=O)C.C(OCC)(=O)C.Cl>CO>[CH2:1]([S:8][CH:9]([CH2:19][N:20]1[CH2:21][CH2:22][S:23][CH2:24][CH2:25]1)[CH2:10][NH2:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 21866389Hydrogen chloride-ethyl acetateHCID 59135685Tert-butyl [2-(benzylthio)-3-thiomorpholinopropyl]carbamate

생성물 1

HCID 574762142-(Benzylthio)-3-thiomorpholinopropan-1-amine수율 91%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of tert-butyl [2-(benzylthio)-3-thiomorpholinopropyl]carbamate (21.46 g) in a mixed solvent of ethyl acetate (60 mL) and methanol (60 mL) was added hydrogen chloride-ethyl acetate solution (120 mL) at 0° C., and the mixture was stirred at room temperature for 4 hr. The reaction solution was concentrated, and the residue was partitioned between ethyl acetate and saturated aqueous potassium carbonate solution. The organic layer was washed with saturated brine, and dried over sodium sulfate, and the solvent was evaporated to give the title compound (14.41 g, yield 91%) as a yellow oil.

후처리

  1. concentrationThe reaction solution was concentrated
  2. customthe residue was partitioned between ethyl acetate and saturated aqueous potassium carbonate solution
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over sodium sulfate
  5. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-5be450cfa2244433aa609ef72c1f5798
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07777047B2

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