Hydrochloric Acid → Cyclohexanecarbaldehyde chlorooxime

HRID 2120087ノート

反応式

HRID 2120087 の反応式
[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

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 638165Cyclohexanecarbaldehyde oximeHCID 23707502Potassium hydroxy sulfite

生成物 1

HCID 74053057Cyclohexanecarbaldehyde chlorooxime

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-74607d4ea3434f80b7bf5633eb364a01
出典データセット
uspto-grants-2004_02
特許番号
US06689778B2

反応ノート

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