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Hydrochloric Acid → 2-Chloro-6-(4,6-dimethoxytriazin-2-yloxy)-benzoic acid

HRID 345269
ノート
印刷プレビュー

反応式

HRID 345269 の反応式
CC([O-])(C)C.[K+].[Cl:7][C:8]1[CH:16]=[CH:15][CH:14]=[C:13]([OH:17])[C:9]=1[C:10]([OH:12])=[O:11].Cl[N:19]1[N:24]=[C:23]([O:25][CH3:26])[CH:22]=[C:21]([O:27][CH3:28])[NH:20]1.Cl>CN(C)C=O.O>[Cl:7][C:8]1[CH:16]=[CH:15][CH:14]=[C:13]([O:17][N:19]2[N:20]=[C:21]([O:27][CH3:28])[CH:22]=[C:23]([O:25][CH3:26])[NH:24]2)[C:9]=1[C:10]([OH:12])=[O:11]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 925912-Chloro-6-hydroxybenzoic acidHCID 221477162-Chloro-4,6-dimethoxy-triazineHCID 23665647Potassium tert-butoxide

生成物 1

HCID 199918532-Chloro-6-(4,6-dimethoxytriazin-2-yloxy)-benzoic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒

反応条件

温度
25 °C

実験手順

At 25° C., 20.2 g of potassium tert-butylate is added in portions to 15.5 g of 2-chloro-6-hydroxybenzoic acid in 50 ml of dimethylformamide. Subsequently, 15.7 g of 2-chloro-4,6-dimethoxytriazine is added. The mixture is stirred for 12 hours at 25° C. and poured into cold water, and the resulting mixture is acidified with hydrochloric acid. Extraction is then carried out with ethyl acetate, and the extract is dried over sodium sulfate and the solvent is removed under reduced pressure. The residue is stirred with a small amount of diethyl ether, followed by filtration. The residue is dried under reduced pressure (m.p. 128°-131° C.).

後処理

  1. extractionExtraction
  2. dry with materialthe extract is dried over sodium sulfate
  3. customthe solvent is removed under reduced pressure
  4. stirringThe residue is stirred with a small amount of diethyl ether
  5. filtrationfollowed by filtration
  6. customThe residue is dried under reduced pressure (m.p. 128°-131° C.)

出典と根拠

ORDレコード
ord-9f0396cf4ca84c5d8c905f274e7561e5
出典データセット
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05057143

反応ノート

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