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Hydrochloric Acid → HCID 89444221, 화합물

HRID 1771725
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HRID 1771725 반응식
[C:1]([C:3]1[CH:4]=[C:5]([CH2:16][NH:17][C:18]2[C:19]([F:32])=[C:20]([CH:28]=[CH:29][C:30]=2[F:31])[O:21][CH2:22][C:23]([O:25]CC)=[O:24])[CH:6]=[C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([F:15])[CH:10]=2)[CH:8]=1)#[N:2].C([O-])([O-])=[O:34].[K+].[K+].OO.Cl>CS(C)=O.O>[C:1]([C:3]1[CH:4]=[C:5]([CH2:16][NH:17][C:18]2[C:19]([F:32])=[C:20]([CH:28]=[CH:29][C:30]=2[F:31])[O:21][CH2:22][C:23]([OH:25])=[O:24])[CH:6]=[C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([F:15])[CH:10]=2)[CH:8]=1)(=[O:34])[NH2:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 11430Potassium CarbonateHCID 89443820HCID 89443820, 화합물

생성물 1

HCID 89444221HCID 89444221, 화합물수율 46.5%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매
HCID 962
Water
용매

실험 절차

To a mixture of ethyl 2-[3-[[3-cyano-5-(3-fluorophenyl)phenyl]methylamino]-2,4-difluoro-phenoxy]acetate (see example 24) (200 mg, 0.45 mmol, 1 eq) and K2CO3 (310 mg, 2.3 mmol, 5 eq) in DMSO (10 mL) at 40° C. was added H2O2 (30% aqueous solution, 10 mL) dropwise. The mixture was stirred for 20 min then cooled to room temperature. Water was added, and the reaction neutralised by addition of diluted HCl. The solid precipitate that formed was collected by filtration, washed with water and dried to give the title compound as white solid (90 mg, 46%).

후처리

  1. customThe solid precipitate that formed
  2. filtrationwas collected by filtration
  3. washwashed with water
  4. customdried

출처 및 근거

ORD 기록
ord-0ff5f1488c264f43a7cb97dc591ec4b5
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09249085B2

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