Hydrochloric Acid → HCID 57747227、化合物

HRID 1163463ノート

反応式

HRID 1163463 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:8]([OH:15])=[C:7]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:6]=1)=[O:4].Cl[C:21]1[CH:22]=[CH:23][C:24]([O:28][C:29]2[CH:34]=[CH:33][C:32]([Cl:35])=[CH:31][C:30]=2[Cl:36])=[C:25]([OH:27])[CH:26]=1.C(=O)([O-])[O-].[K+].[K+].[ClH:43]>O1CCCC1.O>[Cl:43][C:22]1[CH:21]=[CH:26][C:25]([O:27][CH2:2][C:3]([C:5]2[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:8]([OH:15])=[C:7]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:6]=2)=[O:4])=[C:24]([O:28][C:29]2[CH:34]=[CH:33][C:32]([Cl:35])=[CH:31][C:30]=2[Cl:36])[CH:23]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 5564TriclosanHCID 11430Potassium CarbonateHCID 6161612-Bromo-1-[3,5-di(tert-butyl)-4-hydroxyphenyl]ethan-1-one

生成物 1

HCID 57747227HCID 57747227、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 10.0 g (30.5 mmol) of 2-bromo-1-(4-hydroxy-3,5-di-tert-butylphenyl)-ethanone and the 8.8 g (30.5 mmol) of 5-chloro-2-(2,4-di-chloro-phenoxy)-phenol in 50 ml of tetrahydrofuran, 6.3 g (45.7 mmol) of potassium carbonate is added and the mixture is stirred for 4 days at room temperature. After addition of water and adjusting the pH to 5-6 by adding 32% HCl, the mixture is extracted with ethyl acetate. The combined extracts are washed with water, dried and evaporated. Crystallization of the crude product from methanol gives 15.4 g of compound 104, m.p. 111-114° C.

後処理

  1. extractionthe mixture is extracted with ethyl acetate
  2. washThe combined extracts are washed with water
  3. customdried
  4. customevaporated
  5. customCrystallization of the crude product from methanol

出典と根拠

ORDレコード
ord-a92d71a908804df78dbae6c64069ec4b
出典データセット
uspto-grants-2010_10
特許番号
US07820865B2

反応ノート

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