Sodium Hydroxide → 2,3,5-Trichloropyridine

HRID 1704624ノート

反応式

HRID 1704624 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([Cl:9])=[C:4](NN)[N:3]=1.[OH-].[Na+].Cl[O-].[Na+]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([Cl:9])=[CH:4][N:3]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 34261782,3,5-Trichloro-6-hydrazinylpyridineHCID 23665760Sodium Hypochlorite

生成物 1

HCID 276662,3,5-Trichloropyridine

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
88 °C

実験手順

To a stirred mixture of 53.1 grams (0.25 mole) of 2,3,5-trichloro-6-hydrazinopyridine, 250 milliliters of toluene and 500 milliliters of 1.0N sodium hydroxide, under reflux at 88° C., was added over a 20 minute period 350 milliliters of 6.25 percent sodium hypochlorite. After the addition was complete, the mixture was stirred for an additional 10 minutes and then cooled to room temperature. The organic (toluene) phase was separated and concentrated and cooled. The 2,3,5-trichloropyridine was recovered in a yield of 45.3 grams (99.3 percent of theoretical) and had a purity of 97.6 percent. The product was recrystallized from hexane, filtered through activated carbon and was found to melt at 48°-48.5° C. Upon analysis, the product was found to have carbon, hydrogen and nitrogen contents of 32.78, 1.05 and 7.75 percent, respectively, as compared with the theoretical contents of 32.91, 1.10 and 7.68 percent, respectively, as calculated for the above-named compound.

後処理

  1. additionAfter the addition
  2. temperaturecooled to room temperature
  3. customThe organic (toluene) phase was separated
  4. concentrationconcentrated
  5. temperaturecooled
  6. customThe 2,3,5-trichloropyridine was recovered in a yield of 45.3 grams (99.3 percent of theoretical)
  7. customThe product was recrystallized from hexane
  8. filtrationfiltered through activated carbon
  9. customto melt at 48°-48.5° C

出典と根拠

ORDレコード
ord-6a1fafd0f7974249a18a99c1b991a5a4
出典データセット
uspto-grants-1978_11
特許番号
US04127575

反応ノート

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