Ammonium Chloride → HCID 20145559, 화합물

HRID 648676노트

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HRID 648676 반응식
[CH2:1]([Mg]Br)[CH3:2].[O:5]=[CH:6][CH:7]([CH3:12])[CH2:8][C:9]#[C:10][CH3:11].[Cl-].[NH4+]>O1CCCC1>[OH:5][CH:6]([CH:7]([CH3:12])[CH2:8][C:9]#[C:10][CH3:11])[C:1]#[CH:2]

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 20145490HCID 20145490, 화합물HCID 178418443HCID 178418443, 화합물

생성물 1

HCID 20145559HCID 20145559, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

To a solution of 50 ml of 2M ethylmagnesium bromide in tetrahydrofuran at 0° C. was added a solution of 1-oxo-2-methylhex-4-yne in 20 ml of tetrahydrofuran. The mixture was stirred for 11/2 hour at 0° C., poured into saturated ammonium chloride solution, and extracted three times with diethyl ether. The combined extracts were washed with brine, dried over anhydrous sodium sulfate and solvent removed under reduced pressure. The residue was chromatographed on silica gel, eluting with 20% ethyl acetate in hexane, to give 6.0 g of 3-hydroxy-4-methyloct-1,6-diyne, the compound of formula (LXV).

후처리

  1. extractionextracted three times with diethyl ether
  2. washThe combined extracts were washed with brine
  3. dry with materialdried over anhydrous sodium sulfate and solvent
  4. customremoved under reduced pressure
  5. customThe residue was chromatographed on silica gel
  6. washeluting with 20% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-30e959ead8654f209c278b824e62291e
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04735966

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