Hydrochloric Acid → HCID 15228044, 화합물

HRID 1769430노트

반응식

HRID 1769430 반응식
[OH:1][C:2]1[C:3]([F:16])=[C:4]2[C:9](=[O:10])[N:8]([CH3:11])[C:6](=[O:7])[C:5]2=[C:12]([F:15])[C:13]=1[F:14].[C:17](=O)([O-])[O-].[K+].[K+].S(OC)(OC)(=O)=O.Cl>O.CC(C)=O>[CH3:17][O:1][C:2]1[C:3]([F:16])=[C:4]2[C:9](=[O:10])[N:8]([CH3:11])[C:6](=[O:7])[C:5]2=[C:12]([F:15])[C:13]=1[F:14]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 10878985HCID 10878985, 화합물

생성물 1

HCID 15228044HCID 15228044, 화합물

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

The solids from Example 1 were combined with 375 mL of acetone, and 61.08 g of potassium carbonate. With stirring, 55.77 g of dimethyl sulfate was added, and the entire mixture was heated to reflux for 1.5 h. After cooling, 500 mL of water was added and the reaction was acidified with HCl to a pH of 1.0. The mixture was extracted with ethyl acetate and washed with water. After drying with magnesium sulfate and removal of the solvent, 45.08 g of a yellow solid was collected. The solid was assayed as 72% 4-methoxy-3,5,6-trifluoro-N-methylphthalimide. 19F NMR (ppm acetone d6): -133.0 (m), -140.8 (m), -142.6 (m), 1H NMR (ppm acetone d6) 3.05 (s), 4.19 (s).

후처리

  1. temperaturethe entire mixture was heated
  2. temperatureto reflux for 1.5 h
  3. temperatureAfter cooling
  4. extractionThe mixture was extracted with ethyl acetate
  5. washwashed with water
  6. dry with materialAfter drying with magnesium sulfate and removal of the solvent, 45.08 g of a yellow solid
  7. customwas collected

출처 및 근거

ORD 기록
ord-dfa9dfe4a8174900b2178679b95eae94
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05380926

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