Hydrochloric Acid → HCID 178511251、化合物

HRID 247692

反応式

HRID 247692 の反応式
[BH4-].[Na+].[C:3]([C@H:5]1[CH2:10][CH2:9][C@H:8]([CH:11]=[O:12])[CH2:7][CH2:6]1)#[N:4].Cl>CO.C(OCC)C>[OH:12][CH2:11][C@H:8]1[CH2:9][CH2:10][C@H:5]([C:3]#[N:4])[CH2:6][CH2:7]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 178511250HCID 178511250、化合物

生成物 1

HCID 178511251HCID 178511251、化合物収率 98.6%

試薬・触媒・溶媒 1

HCID 21864698Diethyl ether methanol溶媒2 回

反応条件

温度
10 °C

実験手順

A suspension of 829 mg of sodium borohydride in 20 ml of methanol/diethyl ether (vol. 9:1) was treated dropwise within 5 minutes at 0° C. with a solution of 3.0 g of trans-4-cyanocyclohexanecarboxaldehyde in 30 ml of methanol/diethyl ether (vol. 9:1). The reaction mixture was stirred for a further 2 hours at 10° C., then treated with 10 ml of dilute hydrochloric acid and partitioned in methylene chloride/water. The aqueous phase was extracted three times with methylene chloride. The organic phases were washed twice with water, dried over magnesium sulphate, filtered and concentrated. There were obtained 3.0 g (98%) of trans-4-(hydroxymethyl)cyclohexanecarbonitrile as a colourless oil.

後処理

  1. custompartitioned in methylene chloride/water
  2. extractionThe aqueous phase was extracted three times with methylene chloride
  3. washThe organic phases were washed twice with water
  4. dry with materialdried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-25658ef0835a4e17a0aea5913d48d4a1
出典データセット
uspto-grants-1987_11
特許番号
US04709030

関連ノート

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