Dichloromethane → HCID 59589352、化合物

HRID 577012ノート

反応式

HRID 577012 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 diisobutylaluminium 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-6fc69590fd574646930c6c9264b3eabe
出典データセット
uspto-grants-2015_05
特許番号
US09040538B2

反応ノート

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