Dimethylamine → 2-(4-fluorophenyl)-2-(N,N-dimethylamino)acetonitrile

HRID 968078

반응식

HRID 968078 반응식
[CH3:1][NH:2][CH3:3].S(=O)(=O)(O)O.[C-:9]#[N:10].[Na+].[F:12][C:13]1[CH:20]=[CH:19][C:16]([CH:17]=O)=[CH:15][CH:14]=1>O>[F:12][C:13]1[CH:20]=[CH:19][C:16]([CH:17]([N:2]([CH3:3])[CH3:1])[C:9]#[N:10])=[CH:15][CH:14]=1

참가 물질

6

반응물 4

HCID 674DimethylamineHCID 1118Sulfuric AcidHCID 8929Sodium CyanideHCID 680234-Fluorobenzaldehyde

생성물 1

HCID 113098562-(4-fluorophenyl)-2-(N,N-dimethylamino)acetonitrile수율 98.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Into a 1 l four-necked flask equipped with a thermometer, a stirrer and a dropping funnel, 144.5 g (1.6 mol) of a 50.7% dimethylamine aqueous solution and 118.5 g of water were charged, and 159.4 g (0.38 mol) of a 25% of sulfuric acid aqueous solution was dropwise added over a period of 15 minutes at a temperature of not higher than 20° C. with stirring. Then, 67.4 g (1.38 mol) of sodium cyanide was introduced. Then, 155.1 g (1.25 mol) of 4-fluorobenzaldehyde was dropwise added over a period of 20 minutes at from 20 to 30° C. Thereafter, the reaction was carried out at 50° C. for 4 hours. After completion of the reaction, the reaction mixture was subjected to liquid separation. The organic layer was separated and washed with 500 ml of water of 50° C. to obtain 222.8 g (yield: 98.4%) of the desired compound having a purity of 98.4% (by GC analysis).

후처리

  1. additionwere charged
  2. customAfter completion of the reaction
  3. customthe reaction mixture was subjected to liquid separation
  4. customThe organic layer was separated
  5. washwashed with 500 ml of water of 50° C.

출처 및 근거

ORD 기록
ord-812e62ea85a7484cbe5e45f6336653c1
출처 데이터셋
uspto-grants-2005_10
특허 번호
US06956132B2

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