Diethyl Ether → HCID 67076299, 화합물

HRID 2405277노트

반응식

HRID 2405277 반응식
[OH:1][C:2]([CH3:15])([CH3:14])[CH2:3][C:4]1[CH:5]=[C:6]([CH2:10][C:11](O)=[O:12])[CH:7]=[CH:8][CH:9]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].C(OCC)C.CC(=O)OCC>C1COCC1.O>[OH:12][CH2:11][CH2:10][C:6]1[CH:5]=[C:4]([CH2:3][C:2]([CH3:15])([OH:1])[CH3:14])[CH:9]=[CH:8][CH:7]=1

참가 물질

7

반응물 4

HCID 3283Diethyl EtherHCID 8857Ethyl AcetateHCID 21226445Aluminium lithium hydrideHCID 46938719[3-(2-Hydroxy-2-methylpropyl)phenyl]acetic acid

생성물 1

HCID 67076299HCID 67076299, 화합물수율 39.8%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

실험 절차

The compound of step 1 (0.132 g, 0.634 mmol) was dissolved in THF (0.5 ml) and added to a refluxing suspension of lithium aluminium hydride (122 mg, 3.1 mmol) in THF (1 ml). The mixture was stirred for 1 h under reflux and cooled to room temperature. Diethyl ether (6 ml) was added, followed by EA (0.4 ml). Subsequently, water was added slowly until the alumina salts formed a thick slurry from which the supernatant could be decanted easily. The slurry was repeatedly washed with EA, the combined extracts were dried with sodium sulfate and evaporated to dryness. The residue was purified by RP HPLC (water/ACN gradient) to yield 49 mg of the title compound.

후처리

  1. temperatureunder reflux
  2. customformed a thick slurry from which the supernatant
  3. customcould be decanted easily
  4. washThe slurry was repeatedly washed with EA
  5. dry with materialthe combined extracts were dried with sodium sulfate
  6. customevaporated to dryness
  7. customThe residue was purified by RP HPLC (water/ACN gradient)

출처 및 근거

ORD 기록
ord-f1529dff5fba4fffb4dc20bf4af7d10d
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08802720B2

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