Lithium Carbonate → HCID 10516707、化合物

HRID 1596703ノート

反応式

HRID 1596703 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([C:9](=[O:11])[CH3:10])[CH:5]=[CH:6][C:7]=1[OH:8].C(=O)([O-])[O-].[Li+].[Li+].Br[CH2:19][C:20]1[C:25]([F:26])=[CH:24][CH:23]=[CH:22][C:21]=1[F:27]>CN(C)C=O>[OH:1][C:2]1[CH:3]=[C:4]([C:9](=[O:11])[CH3:10])[CH:5]=[CH:6][C:7]=1[O:8][CH2:19][C:20]1[C:25]([F:26])=[CH:24][CH:23]=[CH:22][C:21]=1[F:27]

参加物

5

反応物 3

HCID 11125Lithium CarbonateHCID 145303',4'-DihydroxyacetophenoneHCID 5814352-(Bromomethyl)-1,3-difluorobenzene

生成物 1

HCID 10516707HCID 10516707、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 3′,4′-dihydroxyacetophenone (25.0 g, 164.3 mmol), lithium carbonate (12.1 g, 164.3 mmol), and α-bromo-2,6-difluorotoluene (34.0 g, 164.3 mmol) in dimethyl formamide (400 mL) is stirred at room temperature for 2 days. The mixture is then filtered through celite, and the filtrate is concentrated in vacuo. The residue is diluted with H2O(200 mL), and the mixture is filtered. The collected solid is recrystallized from ethanol to give 3′-hydroxy-4′-(2,6-difluorobenzyloxy)-acetophenone.

後処理

  1. filtrationThe mixture is then filtered through celite
  2. concentrationthe filtrate is concentrated in vacuo
  3. additionThe residue is diluted with H2O(200 mL)
  4. filtrationthe mixture is filtered
  5. customThe collected solid is recrystallized from ethanol

出典と根拠

ORDレコード
ord-4f90ac559ab447b1b1a32448c16bb731
出典データセット
uspto-grants-2001_09
特許番号
US06291530B1

反応ノート

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