Hydrochloric Acid → HCID 13693403, 화합물

HRID 846235노트

반응식

HRID 846235 반응식
[CH3:1][S:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=[O:12])[CH2:10][CH3:11])=[CH:5][CH:4]=1.C([N-]C(C)C)(C)C.[Li+].Br[CH2:22][C:23]([O:25][CH3:26])=[O:24].Cl>C1COCC1.O>[CH3:1][S:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=[O:12])[CH:10]([CH3:11])[CH2:22][C:23]([O:25][CH3:26])=[O:24])=[CH:5][CH:4]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 60984Methyl bromoacetateHCID 8211711-[4-(Methylthio)phenyl]-1-propanoneHCID 2724682Lithium diisopropylamide

생성물 1

HCID 13693403HCID 13693403, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

실험 절차

The ketone from Step A (180 mg) in THF (2 ml) was added to a solution of lithium diisopropylamide (1.1 mmole) in THF (3 ml) at -78° under N2 atmosphere. After 15 minutes methyl bromoacetate (100 μl) was added and the mixture was warmed to ambient temperature and stirred 12 hours. The mixture was poured into water (15 ml) and conc. HCl (2 ml), extracted with CH2Cl2 and the extracts were dried (Na2SO4) evaporated to dryness and the residue purified by chromatography on silica gel to provide the title compound as an oil. NMR (CDCl3): 1.2 (3H, d), 2.55 (3H, s), 2.3-3.1 (2H, m), 3.65 (3H, s), 3.95 (1H, m), 7.3 (2H, d), 7.95 (2H, d).

후처리

  1. extractionextracted with CH2Cl2
  2. dry with materialthe extracts were dried (Na2SO4)
  3. customevaporated to dryness
  4. customthe residue purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-d453165e87fb4a34877f3cb13e11244f
출처 데이터셋
uspto-grants-1992_08
특허 번호
US05135940

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