Sulfuric Acid → HCID 55254012、化合物

HRID 911215ノート

反応式

HRID 911215 の反応式
S(=O)(=O)(O)O.[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:14]=1[CH:21]=[CH:22][N+:23]([O-])=O.[OH-].[Na+]>C1COCC1.O>[F:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:14]=1[CH2:21][CH2:22][NH2:23]

参加物

7

反応物 4

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 66692011HCID 66692011、化合物

生成物 1

HCID 55254012HCID 55254012、化合物収率 100%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

Cautiously add sulfuric acid (14.7 mL, 265 mmol) dropwise at 0° C. to lithium aluminum hydride (1M solution in THF, 565 mL) with efficient stirring. Warm the mixture to ambient temperature for 20 min and then cool back to 0° C. Add a solution of 1-fluoro-4-methoxy-2-(2-nitro-vinyl)-benzene (18.7 g, 95 mmol) in THF (150 mL) by cannula and stir 2.5 h at ambient temperature. Cool the mixture to 0° C., cautiously add water (4.6 mL) followed by 2N aqueous NaOH (4.6 mL) and water (6.5 mL). Remove the precipitate by filtration and evaporate the filtrate to give the desired intermediate (16 g, 100%). MS (ES+) m/z: 170 (+H)+.

後処理

  1. customdropwise at 0° C.
  2. temperaturecool back to 0° C
  3. temperatureCool the mixture to 0° C.
  4. customRemove the precipitate
  5. filtrationby filtration
  6. customevaporate the filtrate

出典と根拠

ORDレコード
ord-7d561f5358c84adb8d24b4a570afcfc4
出典データセット
uspto-grants-2011_09
特許番号
US08022062B2

反応ノート

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