Water → HCID 18796452, 화합물

HRID 582870

반응식

HRID 582870 반응식
[CH3:1][C:2](=[N:4][OH:5])[CH3:3].CC(C)([O-])C.[K+].[Cl:12][C:13]1[CH:20]=[CH:19][C:16]([C:17]#[N:18])=[C:15]([N+]([O-])=O)[CH:14]=1.O>CN(C)C=O>[Cl:12][C:13]1[CH:20]=[CH:19][C:16]([C:17]#[N:18])=[C:15]([O:5][N:4]=[C:2]([CH3:3])[CH3:1])[CH:14]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 67180Acetone, oximeHCID 969244-Chloro-2-nitrobenzonitrileHCID 23665647Potassium tert-butoxide

생성물 1

HCID 18796452HCID 18796452, 화합물수율 65.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In 75 ml of dry N,N-dimethylformamide was dissolved acetone oxime (1.21 g), followed by potassium tertiary butoxide (1.85 g) and stirred under nitrogen. After 30 minutes, 4-chloro-2-nitro-benzonitrile (2.00 g) was added. After an additional 30 minutes the reaction was poured into water (500 ml) and filtered. The solid was collected and dissolved in DCM (250 ml), dried (MgSO4), and concentrated in vacuo. The resulting solid was recrystallized from ethanol to yield 1.5 g of the product, m.p. 83-84° C.

후처리

  1. filtrationfiltered
  2. customThe solid was collected
  3. dissolutiondissolved in DCM (250 ml)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customThe resulting solid was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-b0496799b6cd46ba84d9201c0b9b6e22
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05925766

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