Hydrochloric Acid → HCID 178444539、化合物

HRID 247523

反応式

HRID 247523 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([C@H:12]1[CH2:17][CH2:16][C@H:15]([C:18](O)=[O:19])[CH2:14][CH2:13]1)[CH2:8][CH2:9][CH2:10][CH3:11].Cl>O1CCCC1>[CH2:7]([C@H:12]1[CH2:13][CH2:14][C@H:15]([CH2:18][OH:19])[CH2:16][CH2:17]1)[CH2:8][CH2:9][CH2:10][CH3:11]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 21226445Aluminium lithium hydrideHCID 178444557HCID 178444557、化合物

生成物 1

HCID 178444539HCID 178444539、化合物収率 96%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

3.79 g of lithium aluminium hydride were placed in 100 ml of absolute tetrahydrofuran under argon gasification and treated within 30 minutes with a solution of 19.83 g of trans-4-pentylcyclohexanecarboxylic acid in 100 ml of absolute tetrahydrofuran. After completion of the addition, the mixture was heated to reflux for 1 hour, then cautiously added to 200 ml of 2N hydrochloric acid and extracted three times with 100 ml of diethyl ether each time. The organic phases were washed with 100 ml of saturated sodium carbonate solution, dried over potassium carbonate and concentrated. Distillation of the residue (19.2 g) gave in the main run 17.7 g (96%) of (trans-4-pentylcyclohexyl)methanol as a colourless oil (purity 99.9%); b.p. 89° C./0.2 mmHg.

後処理

  1. additionAfter completion of the addition
  2. temperaturethe mixture was heated
  3. temperatureto reflux for 1 hour
  4. extractionextracted three times with 100 ml of diethyl ether each time
  5. washThe organic phases were washed with 100 ml of saturated sodium carbonate solution
  6. dry with materialdried over potassium carbonate
  7. concentrationconcentrated
  8. distillationDistillation of the residue (19.2 g)

出典と根拠

ORDレコード
ord-88b516eec58444f591eb2bd6058ec7f9
出典データセット
uspto-grants-1987_11
特許番号
US04708441

関連ノート

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