Hydrochloric Acid → HCID 15228044、化合物

HRID 1769430ノート

反応式

HRID 1769430 の反応式
[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]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 10878985HCID 10878985、化合物

生成物 1

HCID 15228044HCID 15228044、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-dfa9dfe4a8174900b2178679b95eae94
出典データセット
uspto-grants-1995_01
特許番号
US05380926

反応ノート

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