Ammonium Chloride → 1-(2-Bromo-thiazol-5-yl)-propan-1-ol

HRID 559687

반응식

HRID 559687 반응식
[Br:1][C:2]1[S:3][C:4]([CH:7]=[O:8])=[CH:5][N:6]=1.[CH2:9]([Mg]Br)[CH3:10].[Cl-].[NH4+]>C1COCC1.C(OCC)C.CCOC(C)=O>[Br:1][C:2]1[S:3][C:4]([CH:7]([OH:8])[CH2:9][CH3:10])=[CH:5][N:6]=1

참가 물질

7

반응물 3

HCID 25517Ammonium ChlorideHCID 27732592-Bromo-1,3-thiazole-5-carbaldehydeHCID 178418443HCID 178418443, 화합물

생성물 1

HCID 584433781-(2-Bromo-thiazol-5-yl)-propan-1-ol

시약·촉매·용매 3

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 2-bromo-thiazole-5-carbaldehyde (1.00 g, 5.21 mmol) in THF (10 mL) was added a 3 M solution of ethylmagnesium bromide (5.00 mL, 15.0 mmol) in diethyl ether. The mixture was stirred for 18 hours. The reaction was poured into saturated aqueous ammonium chloride (100 mL) containing crushed ice and diluted with EtOAc (100 mL). The organic phase was separated, washed with saturated aqueous sodium bicarbonate solution (100 mL), dried over sodium sulfate, filtered and concentrated. The compound was purified by silica gel chromatography eluting with a gradient of 0-100% ethyl acetate in hexanes provided 1-(2-bromo-thiazol-5-yl)-propan-1-ol.

후처리

  1. additioncontaining
  2. customcrushed ice
  3. customThe organic phase was separated
  4. washwashed with saturated aqueous sodium bicarbonate solution (100 mL)
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe compound was purified by silica gel chromatography
  9. washeluting with a gradient of 0-100% ethyl acetate in hexanes

출처 및 근거

ORD 기록
ord-20fafa3892d94be4b24ff1acf6e49953
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063065B2

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