Dichloromethane → 5-Chloro-2-(4-methoxy-phenoxy)-benzaldehyde

HRID 504522

反応式

HRID 504522 の反応式
C([O-])([O-])=O.[Na+].[Na+].[CH3:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1.[Cl:16][C:17]1[CH:18]=[CH:19][C:20](F)=[C:21]([CH:24]=1)[CH:22]=[O:23].C(Cl)Cl>CN(C)C(=O)C.O>[Cl:16][C:17]1[CH:18]=[CH:19][C:20]([O:15][C:12]2[CH:13]=[CH:14][C:9]([O:8][CH3:7])=[CH:10][CH:11]=2)=[C:21]([CH:24]=1)[CH:22]=[O:23]

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 90154-MethoxyphenolHCID 10340Sodium CarbonateHCID 27735865-Chloro-2-fluorobenzaldehyde

生成物 1

HCID 577501175-Chloro-2-(4-methoxy-phenoxy)-benzaldehyde収率 60.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 31374Dimethylacetamide溶媒

実験手順

At the room temperature, anhydrous Na2CO3 (16 g, 0.15 mol) was added into a mixture of 4-methoxy-phenol (14.8 g, 0.12 mol) and 5-chloro-2-fluoro-benzaldehyde (16 g, 0.10 mol) in N,N-Dimethylacetamide (100 mL). After the mixture was refluxed for 3 h, it was cooled to room temperature. Then DCM and water were added. The organic phase was separated, washed with aqueous NaOH (1 N) and brine, dried over anhydrous Na2SO4 and concentrated to give the title compound (16 g).

後処理

  1. temperatureAfter the mixture was refluxed for 3 h
  2. customThe organic phase was separated
  3. washwashed with aqueous NaOH (1 N) and brine
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-7a7dd403969f4058a2dd6a2d4c8f1bf7
出典データセット
uspto-grants-2010_08
特許番号
US07776875B2

関連ノート

読み込み中…