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3-(Methoxymethyl)-4-methylaniline → N-(1-ethylpropyl)-3-(methoxymethyl)-p-toluidine

HRID 1075329
ノート
印刷プレビュー

反応式

HRID 1075329 の反応式
[CH3:1][O:2][CH2:3][C:4]1[CH:5]=[C:6]([CH:8]=[CH:9][C:10]=1[CH3:11])[NH2:7]>C(C(CC)=O)C>[CH2:10]([CH:4]([NH:7][C:6]1[CH:8]=[CH:9][C:10]([CH3:11])=[C:4]([CH2:3][O:2][CH3:1])[CH:5]=1)[CH2:5][CH3:6])[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 127676673-(Methoxymethyl)-4-methylaniline

生成物 1

HCID 12767668N-(1-ethylpropyl)-3-(methoxymethyl)-p-toluidine収率 119%

試薬・触媒・溶媒 1

HCID 7288Ethyl ketone溶媒

実験手順

A mixture of 3-(methoxymethyl)-p-toluidine (9.3 g), 5 angstrom molecular sieves (19 g) and diethyl ketone (40 ml) is stirred at room temperature for 15 hours. The mixture is then filtered. Additional diethyl ketone (10-15 ml) and molecular sieves (10 g) are added to the filtrate. After 40 minutes at 40° to 50° C., the reaction mixture is filtered and then concentrated under vacuum. The crude product (9.0 g) is dissolved in methanol (50 ml) and cooled to 10° C. Sodium borohydrate (3.7 g) and methanol (25 ml) are simultaneously added in small portions. Thirty minutes after these additions, the mixture is acidified with 10% hydrochloric acid while in an ice bath. The mixture is extracted with ether and the ether extract is discarded. The aqueous extract is made alkaline and then extracted with ether. The ether extract is dried over magnesium sulfate and concentrated to yield 8.1 g of an orange oil which is more than 97% homogeneous as estimated by gas-liquid chromatography. Fractional distillation yields a product having a boiling point of 120° to 125° C. at 0.4 to 0.5 mm pressure.

後処理

  1. filtrationThe mixture is then filtered
  2. additionAdditional diethyl ketone (10-15 ml) and molecular sieves (10 g) are added to the filtrate
  3. waitAfter 40 minutes at 40° to 50° C.
  4. filtrationthe reaction mixture is filtered
  5. concentrationconcentrated under vacuum
  6. dissolutionThe crude product (9.0 g) is dissolved in methanol (50 ml)
  7. temperaturecooled to 10° C
  8. additionSodium borohydrate (3.7 g) and methanol (25 ml) are simultaneously added in small portions
  9. customThirty minutes after these additions, the mixture is acidified with 10% hydrochloric acid while in an ice bath
  10. extractionThe mixture is extracted with ether
  11. extractionthe ether extract
  12. extractionThe aqueous extract
  13. extractionextracted with ether
  14. extractionThe ether extract
  15. dry with materialis dried over magnesium sulfate
  16. concentrationconcentrated

出典と根拠

ORDレコード
ord-01fea57a10ef4baebaedc48701c58ef0
出典データセット
uspto-grants-1983_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04395577

反応ノート

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