benzyl N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)carbamate → 4-Chloro-5-(cyclopentyloxy)-2-fluorobenzenamine

HRID 128555

反応式

HRID 128555 の反応式
[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9][CH:10]2[CH2:14][CH2:13][CH2:12][CH2:11]2)=[CH:4][C:3]=1[NH:15]C(=O)OCC1C=CC=CC=1.[H][H]>[Pd].C1(C)C=CC=CC=1>[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9][CH:10]2[CH2:14][CH2:13][CH2:12][CH2:11]2)=[CH:4][C:3]=1[NH2:15]

参加物

5

反応物 2

HCID 19374482benzyl N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)carbamateHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 152793894-Chloro-5-(cyclopentyloxy)-2-fluorobenzenamine収率 99.6%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 1140Toluene溶媒

実験手順

Benzyl N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)carbamate (2.00 g, 5.51 mmol) synthesized as described above, 5% Pd/C (100 mg) as a catalyst, and toluene (15 ml) as a solvent were charged into a 50 cc round-bottom flask, and the inside of the flask was replaced sufficiently with a hydrogen gas. Then, in a hydrogen gas atmosphere, the mixture was thoroughly stirred for 8 hours at 50° C. After completion of the reaction, the catalyst was separated by filtration, the resulting filtrate was dried with anhydrous magnesium sulfate. After separating the drying agent by filtration, the solvent was distilled off under reduced pressure from the filtrate to obtain quantitatively 2-fluoro-4-chloro-5cyclopentyloxyaniline (1.26 g) as a pale brown oily substance. The spectral data and the like are shown in Reference Example 1.

後処理

  1. customAfter completion of the reaction
  2. customthe catalyst was separated by filtration
  3. dry with materialthe resulting filtrate was dried with anhydrous magnesium sulfate
  4. customAfter separating the drying agent
  5. filtrationby filtration
  6. distillationthe solvent was distilled off under reduced pressure from the filtrate

出典と根拠

ORDレコード
ord-15fe274cba2f4116b90fd10b4beba6a7
出典データセット
uspto-grants-1995_11
特許番号
US05464811

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