Hydrochloric Acid → HCID 22406563, 화합물

HRID 440277노트

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HRID 440277 반응식
[C:1]([O:5][C:6]([C:8]1[S:12][C:11]([C:13]([O:15]CC)=[O:14])=[C:10]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])[CH:9]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+].Cl>O1CCOCC1>[C:1]([O:5][C:6]([C:8]1[S:12][C:11]([C:13]([OH:15])=[O:14])=[C:10]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])[CH:9]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 54105850HCID 54105850, 화합물

생성물 1

HCID 22406563HCID 22406563, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
0 °C

실험 절차

A solution of tert-butyl-3-tert-butoxy-2-ethyloxycarbonyl-5-thiophenecarboxylate (11.5 g, 35 mmol) in dioxane with NaOH (2N) (34.5 ml, 70 mmol) was heated for 1.45 hours at 50° C. The mixture was cooled to 0° C., neutralized with HCl (2N), and the solvent evaporated. The residue was triturated with a concentrated aqueous solution of Na2CO3 (400 ml) and ether (200 ml). The aqueous phase was recovered, cooled to 0° C., acidified with HCl (5N) and extracted with ether. After drying, concentration of the etheral phase, and purification by flash silica gel chromatography, the title compound was obtained (3.45 g).

후처리

  1. customthe solvent evaporated
  2. customThe residue was triturated with a concentrated aqueous solution of Na2CO3 (400 ml) and ether (200 ml)
  3. customThe aqueous phase was recovered
  4. temperaturecooled to 0° C.
  5. extractionextracted with ether
  6. customAfter drying
  7. customconcentration of the etheral phase, and purification by flash silica gel chromatography

출처 및 근거

ORD 기록
ord-becb827bde7f4141aae1bc1c3aefa318
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05519015

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