Carbon Dioxide → 3-Cyano-2,4-dichlorobenzoic acid

HRID 1288728

반응식

HRID 1288728 반응식
C([N-]C(C)C)(C)C.[Li+].[Cl:9][C:10]1[CH:17]=[CH:16][CH:15]=[C:14]([Cl:18])[C:11]=1[C:12]#[N:13].[C:19](=[O:21])=[O:20].O>C1COCC1.CCOCC>[C:12]([C:11]1[C:14]([Cl:18])=[C:15]([CH:16]=[CH:17][C:10]=1[Cl:9])[C:19]([OH:21])=[O:20])#[N:13]

참가 물질

7

반응물 4

HCID 280Carbon DioxideHCID 962WaterHCID 3031DichlobenilHCID 2724682Lithium diisopropylamide

생성물 1

HCID 540731813-Cyano-2,4-dichlorobenzoic acid

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of lithium di-isopropylamide (2M in heptane, 25 ml) was added to a solution of 2,6-dichlorobenzonitrile (8.6 g) in THF while maintaining the temperature below -70° C. The mixture was stirred for 1.5 hours then poured onto solid carbon dioxide. It was stirred for 1 hour then diluted with ether. Water was added and the mixture was acidified to pH1. It was extracted with ether, washed with water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness to give 3-cyano-2,4-dichlorobenzoic acid (9.4 g) as a white solid mp 230°-232° C.

후처리

  1. temperaturewhile maintaining the temperature below -70° C
  2. stirringIt was stirred for 1 hour
  3. extractionIt was extracted with ether
  4. washwashed with water
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customThe filtrate was evaporated to dryness

출처 및 근거

ORD 기록
ord-94c6c84eef84410594482a11e584abf1
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05747424

연결된 노트

불러오는 중…