Hydrochloric Acid → HCID 86642481, 화합물

HRID 1689747

반응식

HRID 1689747 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7](Cl)[C:3]=1[CH:4]=[N:5][OH:6].[Cl:12]N1C(=O)CCC1=O.[ClH:20]>CN(C=O)C>[Cl:20][O:6][N:5]=[CH:4][C:3]1[CH:7]=[C:8]([Cl:12])[CH:9]=[CH:10][C:2]=1[Cl:1]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 31398ChlorosuccinimideHCID 91328Benzaldehyde, 2,6-dichloro-, oxime

생성물 1

HCID 86642481HCID 86642481, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2,6-Dichloro-benzaldehyde oxime (7.6 g, 40 mmol) is dissolved in 56 mL of DMF and N-chlorosuccinimide (5.9 g, 44.0 mmol) is added followed by a catalytic amount of HCl gas. The reaction mixture is stirred overnight. The reaction mixture is partitioned between ether and water. The layers are separated and the ether layer is washed with brine and is dried over sodium sulfate. The ether layer is filtered and the solvent is removed under reduced pressure to yield the crude product. The crude product is purified via chromatography using a gradient of 10% ethyl acetate in hexanes to 15% ethyl acetate in hexanes to yield the title compound. 1H-NMR (400 MHz, CDCl3) δ 8.76 (broad, 1H), 7.38-7.26 (m, 3H)

후처리

  1. customThe reaction mixture is partitioned between ether and water
  2. customThe layers are separated
  3. washthe ether layer is washed with brine
  4. dry with materialis dried over sodium sulfate
  5. filtrationThe ether layer is filtered
  6. customthe solvent is removed under reduced pressure
  7. customto yield the crude product
  8. customThe crude product is purified via chromatography

출처 및 근거

ORD 기록
ord-4e199cffcfd24866a61c24e7a6bf75cf
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08153624B2

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