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Potassium ethylxanthate → HCID 88234431, 화합물

HRID 1597431
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HRID 1597431 반응식
[F:1][C:2]([F:19])([F:18])[O:3][C:4]1[CH:17]=[CH:16][C:7]([O:8][C:9]2[CH:15]=[CH:14][C:12](N)=[CH:11][CH:10]=2)=[CH:6][CH:5]=1.N([O-])=O.[Na+].[CH3:24][CH2:25][O:26][C:27]([S-:29])=[S:28].[K+]>Cl.O>[C:27](=[S:28])([O:26][CH2:25][CH3:24])[S:29][C:12]1[CH:14]=[CH:15][C:9]([O:8][C:7]2[CH:16]=[CH:17][C:4]([O:3][C:2]([F:19])([F:18])[F:1])=[CH:5][CH:6]=2)=[CH:10][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 2735045Potassium ethylxanthateHCID 116661924-(4-(Trifluoromethoxy)phenoxy)anilineHCID 23668193Sodium Nitrite

생성물 1

HCID 88234431HCID 88234431, 화합물

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매

실험 절차

Reaction of 4-fluoro-nitrobenzene with 4-trifluoromethoxyphenol in the presence of KOtBu as described in Example 74A, followed by reduction of the nitro group (hydrogen, 10% Pd/C) gave 4-(4-trifluoromethoxyphenoxy)-aniline. The aniline (4.58 g, 17 mmol) was dissolved in conc. HCl (3.1 mL) and ice (4.5 g) cooled to −5 C., then treated with a solution of NaNO2 (1.17 g, 17 mmol) in water (7mL) which was added dropwise. The cold soltion was added to an aqueous (7 mL) solution of potassium xanthate (5.46 g, 34 mmol) and the resulting mixture was heated at 70 C for 2 h, then allowed to cool to rt and partitioned between EtOAc and water. The organic extract was dried (MgSO4), filt ered and concentrated to give the title compound

후처리

  1. additionwas added dropwise
  2. temperaturethe resulting mixture was heated at 70 C for 2 h
  3. custompartitioned between EtOAc and water
  4. extractionThe organic extract
  5. dry with materialwas dried (MgSO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-a8f7d583d7224fd2a082e6da510d371d
출처 데이터셋
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06294573B1

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