Ammonium Chloride → HCID 20145559、化合物

HRID 648676ノート

反応式

HRID 648676 の反応式
[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]

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 20145490HCID 20145490、化合物HCID 178418443HCID 178418443、化合物

生成物 1

HCID 20145559HCID 20145559、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-30e959ead8654f209c278b824e62291e
出典データセット
uspto-grants-1988_04
特許番号
US04735966

反応ノート

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