Ethyl 3-aminocyclohexanecarboxylate → (3-Aminocyclohexyl)methanol

HRID 926724

反応式

HRID 926724 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[NH2:7][CH:8]1[CH2:13][CH2:12][CH2:11][CH:10]([C:14](OCC)=[O:15])[CH2:9]1>C1COCC1>[NH2:7][CH:8]1[CH2:13][CH2:12][CH2:11][CH:10]([CH2:14][OH:15])[CH2:9]1

参加物

4

反応物 2

HCID 418531Ethyl 3-aminocyclohexanecarboxylateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 55290182(3-Aminocyclohexyl)methanol収率 82.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
27.5 °C

実験手順

LAH (107 mg, 2.8 mmol) was added portionwise to a solution of ethyl 3-aminocyclohexanecarboxylate (320 mg, 1.87 mmol) in THF (5 mL) at 0° C. and continued stirring at 25-30° C. for 15 h. The reaction mixture was quenched with aqueous saturated sodium sulphate solution, filtered the solid precipitate, washed the solid with THF; the filtrate collected was concentrated under reduced pressure to afford 200 mg of the title compound.

後処理

  1. customThe reaction mixture was quenched with aqueous saturated sodium sulphate solution
  2. filtrationfiltered the solid precipitate
  3. washwashed the solid with THF
  4. customthe filtrate collected
  5. concentrationwas concentrated under reduced pressure

出典と根拠

ORDレコード
ord-36b5b373046f4b008e295452a1e07d8d
出典データセット
uspto-grants-2016_03
特許番号
US09289419B2

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