Lithium Hydroxide → 2-Cyanoethoxyethylmethylaniline

HRID 1702428

반응식

HRID 1702428 반응식
[OH:1][CH2:2][CH2:3][N:4]([CH3:11])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[OH-].[Li+].[C:14](#[N:17])[CH:15]=[CH2:16]>C(O)(=O)C>[C:14]([CH2:15][CH2:16][O:1][CH2:2][CH2:3][N:4]([CH3:11])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)#[N:17]

참가 물질

5

반응물 3

HCID 3939Lithium HydroxideHCID 7855Acrylonitrile2회HCID 623402-(N-Methylanilino)ethanol

생성물 1

HCID 542300772-Cyanoethoxyethylmethylaniline

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
50 °C

실험 절차

In a one-gallon autoclave was charged 1019 gm (6.75 moles) of hydroxyethylmethylaniline, 3 gm of anhydrous lithium hydroxide, and 532 gm (10 moles) of acrylonitrile. The autoclave was sealed and slowly heated to 50° C. until the initial exotherm was over. The reaction was then heated to 65°-70° C. for 6 hours. The reaction contents were cooled to room temperature and made slightly acidic with acetic acid. The reaction contents were then filtered. The crude filtered reaction product was stripped of all excess acrylonitrile under vacuum (15-30 mm Hg) at a temperature not exceeding 80° C. to give the orange liquid, 2-cyanoethoxyethylmethylaniline. Liquid chromatography showed the product to be about 97.4% purity. The IR, NMR, and GC mass spectra of the product were consistent with 2-cyanoethoxyethylmethylaniline.

후처리

  1. customThe autoclave was sealed
  2. temperatureThe reaction was then heated to 65°-70° C. for 6 hours
  3. customThe reaction contents
  4. temperaturewere cooled to room temperature
  5. customThe reaction contents
  6. filtrationwere then filtered
  7. filtrationThe crude filtered
  8. customreaction product
  9. customexceeding 80° C.

출처 및 근거

ORD 기록
ord-4e6004a95ea4413c926852d1deb39623
출처 데이터셋
uspto-grants-1983_04
특허 번호
US04381265

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