Hydrochloric Acid → HCID 22406563、化合物

HRID 440277ノート

反応式

HRID 440277 の反応式
[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]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 54105850HCID 54105850、化合物

生成物 1

HCID 22406563HCID 22406563、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
0 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-becb827bde7f4141aae1bc1c3aefa318
出典データセット
uspto-grants-1996_05
特許番号
US05519015

反応ノート

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