Hydrochloric Acid → HCID 57983386, 화합물

HRID 1868917노트

반응식

HRID 1868917 반응식
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]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 67099861HCID 67099861, 화합물

생성물 1

HCID 57983386HCID 57983386, 화합물수율 70%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

반응 조건

온도
80 °C

실험 절차

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).

후처리

  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.

출처 및 근거

ORD 기록
ord-c5064b9bad0747b38cea9f8f653ff2e0
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07635715B2

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