Triclosan → Benzyloxy-acetic acid 5-chloro-2-(2,4-dichloro-phenoxy)-phenyl ester

HRID 556118

反応式

HRID 556118 の反応式
[CH:1]1[C:6]([Cl:7])=[CH:5][C:4]([OH:8])=[C:3]([O:9][C:10]2[CH:11]=[CH:12][C:13]([Cl:17])=[CH:14][C:15]=2[Cl:16])[CH:2]=1.C(N(CC)CC)C.[CH2:25]([O:32][CH2:33][C:34](Cl)=[O:35])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>CC(C)=O>[Cl:7][C:6]1[CH:1]=[CH:2][C:3]([O:9][C:10]2[CH:11]=[CH:12][C:13]([Cl:17])=[CH:14][C:15]=2[Cl:16])=[C:4]([O:8][C:34](=[O:35])[CH2:33][O:32][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH:5]=1

参加物

5

反応物 3

HCID 5564TriclosanHCID 8471TriethylamineHCID 177085Benzyloxyacetyl chloride

生成物 1

HCID 57667396Benzyloxy-acetic acid 5-chloro-2-(2,4-dichloro-phenoxy)-phenyl ester

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a mixture of triclosan (7.53 grams, 26 mmol) and triethylamine (8.2 grams, 81 mmol) in acetone (50 mL) at 0° C. was added benzyloxy acetyl chloride (10 grams, 54.2 mmol) drop wise. The reaction mixture was stirred at room temperature for 18 hours. Solids were filtered off and poured onto cold water (100 mL). Crude 4 was extracted into chloroform, washed with 5% sodium bicarbonate solution (2×50 mL), and water (2×50 mL). The chloroform layer was dried over sodium sulphate and distilled off to get crude 4.

後処理

  1. filtrationSolids were filtered off
  2. additionpoured onto cold water (100 mL)
  3. extractionCrude 4 was extracted into chloroform
  4. washwashed with 5% sodium bicarbonate solution (2×50 mL), and water (2×50 mL)
  5. dry with materialThe chloroform layer was dried over sodium sulphate
  6. distillationdistilled off
  7. customto get crude 4

出典と根拠

ORDレコード
ord-9316240e3078474c9d0243d9cd33afdd
出典データセット
uspto-grants-2011_11
特許番号
US08053591B2

関連ノート

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