Acetic Acid → HCID 67467860、化合物

HRID 509283

反応式

HRID 509283 の反応式
[OH:1][C:2]1([CH3:9])[CH2:7][CH2:6][C:5](=O)[CH2:4][CH2:3]1.[CH:10]1([NH2:13])[CH2:12][CH2:11]1.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+].C(O)(=O)C.[OH-].[Na+]>ClCCCl>[CH:10]1([NH:13][CH:5]2[CH2:6][CH2:7][C:2]([CH3:9])([OH:1])[CH2:3][CH2:4]2)[CH2:12][CH2:11]1

参加物

7

反応物 5

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 285394-Hydroxy-4-methylcyclohexanoneHCID 69828CyclopropylamineHCID 5049666Sodium triacetoxyborohydride

生成物 1

HCID 67467860HCID 67467860、化合物収率 72%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

4-Hydroxy-4-methylcyclohexanone (440 mg, 3.43 mmol) was dissolved in 1,2-dichloroethane (15 ml), followed by sequential addition of cyclopropylamine (0.26 ml, 3.78 mmol), NaBH(OAc)3 (1.16 g, 5.49 mmol), and acetic acid (0.20 ml, 3.43 mmol), and then the resulting mixture was stirred at room temperature under nitrogen stream for 20 hours. The resulting reaction liquid was neutralized by addition of 10% aqueous NaOH solution, and extracted with 5% MeOH/MC (15 ml×4). The organic layer was dried over anhydrous sodium sulfate, followed by filtration, concentration, and vacuum drying, to obtain 417 mg of yellow solid (72%).

後処理

  1. customThe resulting reaction liquid
  2. extractionextracted with 5% MeOH/MC (15 ml×4)
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. filtrationfollowed by filtration, concentration, and vacuum
  5. customdrying

出典と根拠

ORDレコード
ord-2220842ccbbd4c5480c96cb0cd86947b
出典データセット
uspto-grants-2015_08
特許番号
US09096571B2

関連ノート

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