HCID 20441164、化合物 → HCID 20441130、化合物

HRID 1632909ノート

反応式

HRID 1632909 の反応式
[O:1]1[CH2:6][CH2:5][CH2:4][O:3][CH:2]1[CH2:7][NH2:8].[N+:9]([C:12]1[CH:23]=[CH:22][C:21]([O:24][C:25]2[CH:30]=[CH:29][C:28]([F:31])=[CH:27][C:26]=2[C:32]#[N:33])=[CH:20][C:13]=1[O:14][CH:15]([CH3:19])[C:16](Cl)=[O:17])([O-:11])=[O:10]>C(Cl)Cl>[O:1]1[CH2:6][CH2:5][CH2:4][O:3][CH:2]1[CH2:7][NH:8][C:16](=[O:17])[CH:15]([O:14][C:13]1[CH:20]=[C:21]([O:24][C:25]2[CH:30]=[CH:29][C:28]([F:31])=[CH:27][C:26]=2[C:32]#[N:33])[CH:22]=[CH:23][C:12]=1[N+:9]([O-:11])=[O:10])[CH3:19]

参加物

4

反応物 2

HCID 20441164HCID 20441164、化合物HCID 212488031-(1,3-Dioxan-2-yl)methanamine

生成物 1

HCID 20441130HCID 20441130、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
-15 °C

実験手順

N-(1,3-Dioxan-2-ylmethyl)amine (0.015 mole) triethylamine (5 ml) and methylene chloride (50 ml) are charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and addition funnel. The reaction mixture is cooled to about -15° C. and a solution of 2-[2-nitro-5-(2-cyano-4-fluorophenoxy)phenoxy]propionyl chloride (0.01 mole) in methylene chloride (50 ml) is added dropwise with stirring. After the addition is completed the reaction mixture is allowed to warm to room temperature with continued stirring. After this time the mixture is transferred to a separatory funnel and is washed with water and dilute aqueous sodium bicarbonate. The washed solution is then dried, filtered and stripped of solvent leaving a residue. The residue is then recrystallized from a toluene/hexane mixture to yield the desired product N-(1,3-dioxan-2-ylmethyl)-2-[2-nitro-5-(2-cyano-4-fluorophenoxy)phenoxy]propionamide.

後処理

  1. customequipped with a mechanical stirrer
  2. additionthermometer and addition funnel
  3. additionAfter the addition
  4. temperatureto warm to room temperature with continued stirring
  5. customAfter this time the mixture is transferred to a separatory funnel
  6. washis washed with water and dilute aqueous sodium bicarbonate
  7. customThe washed solution is then dried
  8. filtrationfiltered
  9. customleaving a residue
  10. customThe residue is then recrystallized from a toluene/hexane mixture

出典と根拠

ORDレコード
ord-000c56d7b5b04a1f8f921fb5630859e8
出典データセット
uspto-grants-1984_10
特許番号
US04478634

反応ノート

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