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Potassium ethylxanthate → HCID 88234431、化合物

HRID 1597431
ノート
印刷プレビュー

反応式

HRID 1597431 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

HCID 88234431HCID 88234431、化合物

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-a8f7d583d7224fd2a082e6da510d371d
出典データセット
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06294573B1

反応ノート

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