Lithium Carbonate → HCID 10516707, 화합물

HRID 1596703

반응식

HRID 1596703 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 10516707HCID 10516707, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4f90ac559ab447b1b1a32448c16bb731
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06291530B1

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