Dichloromethane → HCID 59589352、化合物

HRID 630053ノート

反応式

HRID 630053 の反応式
[Cl:1][C:2]1[CH:11]=[CH:10][C:9]([CH2:12][N:13]([CH2:16][CH3:17])[CH2:14][CH3:15])=[CH:8][C:3]=1[C:4](OC)=[O:5].[H-].C([Al+]CC(C)C)C(C)C.[C@H](O)(C([O-])=O)[C@@H](O)C([O-])=O.[Na+].[K+].ClCCl>C1COCC1>[Cl:1][C:2]1[CH:11]=[CH:10][C:9]([CH2:12][N:13]([CH2:14][CH3:15])[CH2:16][CH3:17])=[CH:8][C:3]=1[CH2:4][OH:5]

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 9357Potassium Sodium TartrateHCID 21225700DiisobutylaluminumhydrideHCID 59589465HCID 59589465、化合物

生成物 1

HCID 59589352HCID 59589352、化合物収率 85%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of methyl 2-chloro-5-[(diethylamino)methyl]benzoate (3.97 g, 15.5 mmol) in anhydrous THF (100 mL) was added a solution of diisobutylaluminum hydride (1 M in toluene, 35 mL, 35 mmol). The reaction mixture was stirred at room temperature for 90 minutes. A Rochelle's salt solution (200 mL) and dichloromethane (200 mL) were added. The resultant mixture was stirred at room temperature for 2 hours. The organic layer was recovered, dried over MgSO4, filtered, evaporated, and dried in vacuo, affording {2-chloro-5-[(diethylamino)methyl]phenyl}methanol (3.0 mg, 85% yield). The product was used without further purification.

後処理

  1. customThe organic layer was recovered
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. customevaporated
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-5aada7737db04a63b17691010d0ace05
出典データセット
uspto-grants-2016_04
特許番号
US09315521B2

反応ノート

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