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1-Bromo-3-chloropropane → HCID 86709383, 화합물

HRID 2172210
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HRID 2172210 반응식
Br[CH2:2][CH2:3][CH2:4][Cl:5].[F:6][C:7]([F:17])([F:16])[O:8][C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1.C(=O)([O-])[O-].[K+].[K+]>CN1C(=O)CCC1>[Cl:5][CH2:4][CH2:3][CH2:2][O:15][C:12]1[CH:13]=[CH:14][C:9]([O:8][C:7]([F:6])([F:16])[F:17])=[CH:10][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 70015p-(Trifluoromethoxy)phenol

생성물 1

HCID 86709383HCID 86709383, 화합물수율 99.9%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

1-Bromo-3-chloropropane (2.37 ml, 24 mmol), 4-(trifluoromethoxy)phenol (3.56 g, 20 mmol) and potassium carbonate (4.15 g, 30 mmol) were stirred in NMP (30 ml) overnight. After removing potassium carbonate by filtration, water was added to the mixture, followed by extraction with ethyl acetate. The organic layer was washed with water and dried over sodium sulfate. The solvent was distilled off, and the residue was fractionated and purified by silica gel column chromatography (hexane:ethyl acetate=89:11) to afford the title compound as a colorless oil (5.09 g, yield 99%).

후처리

  1. customAfter removing potassium carbonate
  2. filtrationby filtration, water
  3. additionwas added to the mixture
  4. extractionfollowed by extraction with ethyl acetate
  5. washThe organic layer was washed with water
  6. dry with materialdried over sodium sulfate
  7. distillationThe solvent was distilled off
  8. custompurified by silica gel column chromatography (hexane:ethyl acetate=89:11)

출처 및 근거

ORD 기록
ord-15de6ca750fd47a2927b51c37d5715e7
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09051333B2

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