Water → HCID 54343145, 화합물

HRID 620928노트

반응식

HRID 620928 반응식
Cl[CH2:2][C:3](=[O:18])[C:4]([NH:7][C:8](=[O:17])[C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[C:11]([Cl:16])[CH:10]=1)([CH3:6])[CH3:5].[C-:19]#[N:20].[Na+].O.C(Cl)Cl>C(#N)C.C1OCCOCCOCCOCCOCCOC1>[C:19]([CH2:2][C:3](=[O:18])[C:4]([NH:7][C:8](=[O:17])[C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[C:11]([Cl:16])[CH:10]=1)([CH3:6])[CH3:5])#[N:20]

참가 물질

7

반응물 4

HCID 962WaterHCID 6344DichloromethaneHCID 8929Sodium CyanideHCID 54029353HCID 54029353, 화합물

생성물 1

HCID 54343145HCID 54343145, 화합물수율 43%

시약·촉매·용매 2

HCID 2855718-Crown-6촉매HCID 6342Acetonitrile용매

실험 절차

N-(3'-chloro-1',1'-dimethylacetonyl)-3,5-dichlorobenzamide (30 gm, 0.0972 m), sodium cyanide (15 gm, 0.306 m) and 18-crown-6 (1 gm) were dissolved in 300 ml of acetonitrile in a round bottom flask under a nitrogen atmosphere. The mixture was heated to reflux for about 4 hours. The contents of the flask were then cooled and transferred to a separatory funnel along with 100 ml of water and 500 ml of methylene chloride and mixed well. The aqueous layer was discarded and the organic layer was washed sequentially with water and brine, dried and the solvents stripped off to yield 12.5 gm of the product after recrystallization from methylene chloride and hexane.

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux for about 4 hours
  3. temperatureThe contents of the flask were then cooled
  4. additionmixed well
  5. washthe organic layer was washed sequentially with water and brine
  6. customdried

출처 및 근거

ORD 기록
ord-39846c1738f4450390c5a43c91f59f8e
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04822902

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