Cyclohexylamine → HCID 13746371、化合物

HRID 1195606ノート

反応式

HRID 1195606 の反応式
C1(O[C:8](=[O:19])[NH:9][O:10][C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([Cl:17])[C:12]=2[Cl:18])C=CC=CC=1.[CH:20]1([NH2:26])[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1>C(OCC)(=O)C>[CH:20]1([NH:26][C:8]([NH:9][O:10][C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([Cl:17])[C:12]=2[Cl:18])=[O:19])[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1

参加物

4

反応物 2

HCID 7965CyclohexylamineHCID 13746370Phenyl (2,3-dichlorophenoxy)carbamate

生成物 1

HCID 13746371HCID 13746371、化合物収率 69.9%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

4.00 g (13.4 mmole) of N-(2,3-dichlorophenoxy)carbamic acid phenyl ester synthesized in Reference Example 1 was dissolved in 60 ml of ethyl acetate. 3.32 g (33.5 mmole) of cyclohexylamine was added thereto, and the mixture was reacted at 60° C. for 12 hours. The reaction mixture was cooled to room temperature, and after an addition of 100 ml of ethyl acetate, it was washed with a 3% sodium hydroxide aqueous solution and then with a saturated sodium chloride solution, and then dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure, and the residue was recrystallized from ethyl acetate-hexane, whereby 2.84 g of the desired product was obtained as light brown crystals (yield: 70%).

後処理

  1. customthe mixture was reacted at 60° C. for 12 hours
  2. washwas washed with a 3% sodium hydroxide aqueous solution
  3. dry with materialwith a saturated sodium chloride solution, and then dried over anhydrous magnesium sulfate
  4. distillationEthyl acetate was distilled off under reduced pressure
  5. customthe residue was recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-3031bea09f394095b134301b1a64c42b
出典データセット
uspto-grants-1992_05
特許番号
US05112385

反応ノート

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