Lithium Hydroxide → 2-Cyanoethoxyethylmethylaniline

HRID 1702428

反応式

HRID 1702428 の反応式
[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]

参加物

5

反応物 3

HCID 3939Lithium HydroxideHCID 7855Acrylonitrile2 回HCID 623402-(N-Methylanilino)ethanol

生成物 1

HCID 542300772-Cyanoethoxyethylmethylaniline

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-4e6004a95ea4413c926852d1deb39623
出典データセット
uspto-grants-1983_04
特許番号
US04381265

関連ノート

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