Diethyl Ether → HCID 67076299、化合物

HRID 2094737ノート

反応式

HRID 2094737 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 67076299HCID 67076299、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0b8887c780764bb2b77b6018e4438221
出典データセット
uspto-grants-2013_05
特許番号
US08445530B2

反応ノート

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