Hydrochloric Acid → 33228-49-8

HRID 867353ノート

反応式

HRID 867353 の反応式
[CH2:1]([C:7]1[CH:13]=[CH:12][C:10]([NH2:11])=[CH:9][CH:8]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].Cl.[N:15]([O-])=O.[Na+].[OH-].[Na+].[C:21]1([OH:27])[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>O>[OH:27][C:21]1[CH:26]=[CH:25][C:24]([N:15]=[N:11][C:10]2[CH:9]=[CH:8][C:7]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])=[CH:13][CH:12]=2)=[CH:23][CH:22]=1

参加物

7

反応物 5

HCID 313Hydrochloric Acid2 回HCID 996PhenolHCID 14798Sodium HydroxideHCID 363824-HexylanilineHCID 23668193Sodium Nitrite

生成物 1

HCID 13570282833228-49-8収率 120.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

30.1 g (0.17 M) of 4-hexylaniline was cooled to 0° C. or below, 85 gof 10% aqueous hydrochloric acid solution was added, and then a solution of11.6 g of sodium nitrite in 68 g of water was added. During the addition, the mixture was cooled so as not to exceed 0° C. After the addition, the mixture was allowed to react for 30 minutes, transferred into a dropping funnel and added dropwise into 170 g of an 8% NaOH aqueoussolution containing 16 g of phenol held at 5° C. or below. After theaddition, the mixture was stirred for 0.5 hour, and then 10% hydrochloric acid aqueous solution was added thereto until a pH of 5-6 to precipitate the reaction product. The precipitate was separated by filtration, washed with water and dried overnight under reduced pressure. After the drying, the product was washed with 500 ml of petroleum ether and further dried under reduced pressure to obtain 29.6 g (0.10M) of 4-hydroxy-4'-hexylazobenzene. The yield was 59%.

後処理

  1. additionDuring the addition
  2. temperaturethe mixture was cooled so as not
  3. customto exceed 0° C
  4. additionAfter the addition
  5. customto react for 30 minutes
  6. customtransferred into a dropping funnel
  7. customheld at 5° C. or below
  8. customuntil a pH of 5-6 to precipitate the reaction product
  9. customThe precipitate was separated by filtration
  10. washwashed with water
  11. customdried overnight under reduced pressure
  12. washAfter the drying, the product was washed with 500 ml of petroleum ether
  13. customfurther dried under reduced pressure

出典と根拠

ORDレコード
ord-e136669893644a538cc9a539a116c1bd
出典データセット
uspto-grants-1988_10
特許番号
US04775223

反応ノート

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