Sulfuric Acid → HCID 55254012, 화합물

HRID 911215노트

반응식

HRID 911215 반응식
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]

참가 물질

7

반응물 4

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 66692011HCID 66692011, 화합물

생성물 1

HCID 55254012HCID 55254012, 화합물수율 100%

시약·촉매·용매 2

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-7d561f5358c84adb8d24b4a570afcfc4
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022062B2

반응 노트

불러오는 중…