Hydrochloric Acid → Cyclohexanecarbaldehyde chlorooxime

HRID 2120087노트

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HRID 2120087 반응식
[CH:1]1([CH:7]=[N:8][OH:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[ClH:10].OOS([O-])=O.[K+]>CN(C=O)C>[Cl:10][O:9][N:8]=[CH:7][CH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 638165Cyclohexanecarbaldehyde oximeHCID 23707502Potassium hydroxy sulfite

생성물 1

HCID 74053057Cyclohexanecarbaldehyde chlorooxime

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of the oxime formed in Example 1 (1 g, 8.25 mmol) in HCl (0.5 M in dioxane; 18.16 ml, 9.08 mmol) and DMF (40 ml) was added oxone (2.79 g, 4.54 mmol) and the resulting mixture was stirred overnight at room temperature. The reaction was partitioned between diethylether and water and the layers were separated. The organic layer was washed with saturated ammonium chloride, dried over sodium sulfate, then concentrates in vacuo using a room temperature water bath. The resulting low boiling liquid was carried on directly to the next step. 1H NMR (CDCl3) δ 1.0-2.2 (m, 10H), 2.35 (m, 1H), 7.8 (bd, 1H).

후처리

  1. customThe reaction was partitioned between diethylether and water
  2. customthe layers were separated
  3. washThe organic layer was washed with saturated ammonium chloride
  4. dry with materialdried over sodium sulfate
  5. customusing a room temperature

출처 및 근거

ORD 기록
ord-74607d4ea3434f80b7bf5633eb364a01
출처 데이터셋
uspto-grants-2004_02
특허 번호
US06689778B2

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