Hydrochloric Acid → 2-Propenamide, N-(2-ethylhexyl)-

HRID 364676

반응식

HRID 364676 반응식
[CH2:1]([CH:3]([CH2:6][CH2:7][CH2:8][CH3:9])[CH2:4][NH2:5])[CH3:2].[C:10]([CH:14]1CC2O[CH:15]1C=C2)(OC)=[O:11].Cl.C(Cl)Cl>O>[CH2:1]([CH:3]([CH2:6][CH2:7][CH2:8][CH3:9])[CH2:4][NH:5][C:10](=[O:11])[CH:14]=[CH2:15])[CH3:2]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 77192-EthylhexylamineHCID 12271748Methyl 7-oxabicyclo[2.2.1]hept-5-ene-2-carboxylate

생성물 1

HCID 104649792-Propenamide, N-(2-ethylhexyl)-

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
140 °C

실험 절차

7.2 parts 30% methanolic Na-methylate solution are added to 64.5 parts 2-ethylhexylamine. 77 parts 2-carbomethoxy-7-oxabicyclo(2,2,1)hept-5-ene are added drop-wise at 30° to 35° C. during cooling. The reaction medium is then stirred for 15 hours and neutralised with 4 parts concentrated hydrochloric acid. 100 parts methylene chloride and 50 parts water are added, the organic phase separated off, and the aqueous phase extracted twice with 25 ml methylene chloride in each instance. The combined organic phases are reduced in a rotary evaporator at a bath temperature of 90° C. and a vacuum of 20 Torr. The residue is heated under a high vacuum to 110° to 120° C. (bath temperature 140° C.). On conclusion of the furane separation, the sedimentation temperature increases and the product distills over. 66.6 parts N(2-ethylhexyl)acrylamide with a boiling point of 123° C. at 0.4 Torr are obtained.

후처리

  1. temperatureduring cooling
  2. customthe organic phase separated off
  3. extractionthe aqueous phase extracted twice with 25 ml methylene chloride in each instance
  4. customThe combined organic phases are reduced in a rotary evaporator at a bath temperature of 90° C.
  5. customOn conclusion of the furane separation
  6. temperaturethe sedimentation temperature increases
  7. distillationthe product distills over

출처 및 근거

ORD 기록
ord-40c98682a7514ca69888367bd7e5dca6
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04605740

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