Hydrochloric Acid → 3-Bromo-6-methoxy-2-methylbenzoic acid

HRID 611714

反応式

HRID 611714 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([O:14][CH3:15])=[C:6]([C:12]=1[CH3:13])[C:7]([O:9]CC)=[O:8].C(O)C.[OH-].[Na+].Cl>O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([O:14][CH3:15])=[C:6]([C:12]=1[CH3:13])[C:7]([OH:9])=[O:8]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 11022052Ethyl 3-bromo-6-methoxy-2-methylbenzoate

生成物 1

HCID 27529923-Bromo-6-methoxy-2-methylbenzoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A mixture of 6A (9.8 g, 34.1 mmol), water (40 ml), ethanol (80 ml) and sodium hydroxide (2.7 g, 68.3 mmol) is heated under reflux with stirring for 42 hours. The reaction mixture is diluted with water (80 ml), acidified with concentrated hydrochloric acid and extracted with dichloromethane. The organic phase is separated and concentrated. The solid material is collected by filtration, washed with water and dried yielding off-white crystals, 5.4 g (61%), mp 81-83° C.

後処理

  1. temperatureis heated
  2. temperatureunder reflux
  3. extractionextracted with dichloromethane
  4. customThe organic phase is separated
  5. concentrationconcentrated
  6. filtrationThe solid material is collected by filtration
  7. washwashed with water
  8. customdried
  9. customyielding off-white crystals, 5.4 g (61%), mp 81-83° C.

出典と根拠

ORDレコード
ord-0b0cb8a088954f98aaf85400530f0717
出典データセット
uspto-grants-1999_12
特許番号
US06001883

関連ノート

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