Hydrochloric Acid → 3,3-difluoro-3,4-dihydro-2H-thieno[3,4-b][1,4]-dioxepine-6,8-dicarboxylic acid

HRID 1794557ノート

反応式

HRID 1794557 の反応式
C([O:3][C:4]([C:6]1[S:7][C:8]([C:18]([O:20]CC)=[O:19])=[C:9]2[C:15]=1[O:14][CH2:13][C:12]([F:17])([F:16])[CH2:11][O:10]2)=[O:5])C.[OH-].[Na+].Cl>C(O)C>[F:17][C:12]1([F:16])[CH2:11][O:10][C:9]2=[C:8]([C:18]([OH:20])=[O:19])[S:7][C:6]([C:4]([OH:5])=[O:3])=[C:15]2[O:14][CH2:13]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 695461653,3-difluoro-3,4-dihydro-2H-thieno[3,4-b][1,4]-dioxepine-6,8-dicarboxylic acid diethyl ester

生成物 1

HCID 222221443,3-difluoro-3,4-dihydro-2H-thieno[3,4-b][1,4]-dioxepine-6,8-dicarboxylic acid収率 71,571.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

953 mg (3.67 mmol) of 3,3-Difluoro-3,4-dihydro-2H-thieno[3,4-b][1,4]-dioxepine-6,8-dicarboxylic acid diethyl ester in 75 mL of ethanol was mixed with 1.10 g (27.5 mmol) of sodium hydroxide granules and stirred for 2 hours under nitrogen at room temperature. After acidifying the resulting mixture with 2N hydrochloric acid, the ethanol was largely evaporated off using a rotary evaporator, the solids filtered off, the filtrate washed three times with water and then dried in air. 736 g of 3,3-difluoro-3,4-dihydro-2H-thieno[3,4-b][1,4]-dioxepine-6,8-dicarboxylic acid was obtained corresponding to a yield of 92% yield with a melting point of 288–293° C., as characterized by:

後処理

  1. customthe ethanol was largely evaporated off
  2. customa rotary evaporator
  3. filtrationthe solids filtered off
  4. washthe filtrate washed three times with water
  5. customdried in air

出典と根拠

ORDレコード
ord-ab0963cecf7949d4b8dab9acf926791e
出典データセット
uspto-grants-2006_04
特許番号
US07022811B2

反応ノート

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