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

HRID 1949181

반응식

HRID 1949181 반응식
[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

참가 물질

5

반응물 3

HCID 5564TriclosanHCID 8471TriethylamineHCID 177085Benzyloxyacetyl chloride

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-99aa6b9310a04be393bfc254b99f5a32
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399696B2

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