Hydrochloric Acid → HCID 57983386、化合物

HRID 1868917ノート

反応式

HRID 1868917 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-c5064b9bad0747b38cea9f8f653ff2e0
出典データセット
uspto-grants-2009_12
特許番号
US07635715B2

反応ノート

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