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Water → HCID 89619306, 화합물

HRID 1525668
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HRID 1525668 반응식
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][CH2:7][C:8]2[CH:18]=[CH:17][C:11]([C:12]([O:14]CC)=[O:13])=[CH:10][CH:9]=2)=[CH:4][C:3]=1[C:21]([F:24])([F:23])[F:22].O.[OH-].[Na+]>CO.CCOC(C)=O.Cl>[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][CH2:7][C:8]2[CH:9]=[CH:10][C:11]([C:12]([OH:14])=[O:13])=[CH:17][CH:18]=2)=[CH:4][C:3]=1[C:21]([F:22])([F:23])[F:24]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 89619235HCID 89619235, 화합물

생성물 1

HCID 89619306HCID 89619306, 화합물수율 86%

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 887Methanol용매
HCID 8857
Ethyl Acetate
용매

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온도
55 °C

실험 절차

To a solution of ethyl 4-{[4-chloro-3-(trifluoromethyl)phenoxy]methyl}benzoate (Preparation 17, 350 mg, 0.98 mmol) in methanol (8.0 mL) was added water (2 mL) followed by sodium hydroxide (400 mg, 9.8 mmol). The reaction mixture was heated to 55° C. for 3 hours, then cooled and diluted with EtOAc (50 mL) and 2M HCl (50 mL). The aqueous layer was separated and washed with EtOAc (2×50 mL). The combined organic layers were dried over magnesium sulfate, filtered and concentrated in vacuo to yield a white solid as the title compound (276 mg, 86%).

후처리

  1. temperaturecooled
  2. customThe aqueous layer was separated
  3. washwashed with EtOAc (2×50 mL)
  4. dry with materialThe combined organic layers were dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-5d3bfa579ed84828a67becd97ac7f9f3
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09085517B2

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