Hydrochloric Acid → HCID 57983386、化合物

HRID 2078325ノート

反応式

HRID 2078325 の反応式
Cl.[Br:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([CH3:21])([CH3:20])[C:8](=[O:19])[C:9](C(OCC)=O)=[C:10]2[OH:13])=[CH:5][CH:4]=1>C(O)(C(F)(F)F)=O>[Br:2][C:3]1[CH:12]=[C:11]2[C:6](=[CH:5][CH:4]=1)[C:7]([CH3:21])([CH3:20])[C:8](=[O:19])[CH:9]=[C:10]2[OH:13]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 67099861HCID 67099861、化合物

生成物 1

HCID 57983386HCID 57983386、化合物収率 70%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
80 °C

実験手順

Concentrated aqueous HCl (36.5-37.5%, 10 mL) was added to a solution of ethyl 7-bromo-1-hydroxy-4,4-dimethyl-3-oxo-3,4-dihydronaphthalene-2-carboxylate (1.40 g, 4 mmol) in TFA (10 mL). The mixture was heated to 80° C. for 18 hours. The solvent was then removed under reduced pressure, and the residue was rinsed with water and diethyl ether. The remaining solids were dried in vacuo at 50° C. to afford the title compound in 70% yield. 1H-NMR (300 MHz, DMSO-d6) δ ppm 7.98 (1H, d, J=1.9 Hz), 7.75 (1H, dd, J=2.0, 8.5 Hz), 7.67 (1H, br. d, J˜8.0 Hz), 5.64 (1H, s), 2.51 (6H, m). MS (m/z not observed).

後処理

  1. customThe solvent was then removed under reduced pressure
  2. washthe residue was rinsed with water and diethyl ether
  3. customThe remaining solids were dried in vacuo at 50° C.

出典と根拠

ORDレコード
ord-797be1b8f6c4414da9513405686e9bdf
出典データセット
uspto-grants-2011_04
特許番号
US07928139B2

反応ノート

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