Hydrochloric Acid → HCID 10568313、化合物

HRID 862075ノート

反応式

HRID 862075 の反応式
[Br:1][C:2]1[C:3]([Cl:24])=[CH:4][C:5]([O:20]COC)=[C:6]([CH:19]=1)[C:7]([C:9]1[C:14]([O:15]COC)=[CH:13][CH:12]=[CH:11][N:10]=1)=[O:8].Cl>CO>[Br:1][C:2]1[C:3]([Cl:24])=[CH:4][C:5]([OH:20])=[C:6]([CH:19]=1)[C:7]([C:9]1[C:14]([OH:15])=[CH:13][CH:12]=[CH:11][N:10]=1)=[O:8]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 108357432-(5-Bromo-4-chloro-2-methoxymethoxybenzoyl)-3-methoxymethoxypyridine

生成物 1

HCID 10568313HCID 10568313、化合物収率 97.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

To a solution of 2-(5-bromo-4-chloro-2-methoxymethoxybenzoyl)-3-methoxymethoxypyridine (7.73 g) in methanol (250 ml) was added hydrochloric acid (12.5 ml), which was stirred for 5 hours at 50° C. Methanol was distilled off under reduced pressure. To the residue was added ethyl acetate (5 ml), which was poured into water. Crystalline precipitate then formed was collected by filtration, washed with ethyl acetate 10 and dried to give 2-(5-bromo-4-chloro-2-hydroxybenzoyl)-3-hydroxypyridine (5.95 g) (Compound A-8).

後処理

  1. distillationMethanol was distilled off under reduced pressure
  2. additionTo the residue was added ethyl acetate (5 ml), which
  3. additionwas poured into water
  4. customCrystalline precipitate then formed
  5. filtrationwas collected by filtration
  6. washwashed with ethyl acetate 10
  7. customdried

出典と根拠

ORDレコード
ord-cb31bb7f5900478c8ebe2f3eca5bbab7
出典データセット
uspto-grants-1998_02
特許番号
US05716971

反応ノート

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