Hydrochloric Acid → 2-(3-Fluoro-2-methyl-benzyl)-3-phenyl-indolizine-1-carboxylic acid

HRID 1963093ノート

反応式

HRID 1963093 の反応式
C[O:2][C:3]([C:5]1[C:6]([CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[C:23]([F:27])[C:22]=2[CH3:28])=[C:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:8]2[C:13]=1[CH:12]=[CH:11][CH:10]=[CH:9]2)=[O:4].[OH-].[Na+].Cl>O1CCOCC1>[F:27][C:23]1[C:22]([CH3:28])=[C:21]([CH:26]=[CH:25][CH:24]=1)[CH2:20][C:6]1[C:5]([C:3]([OH:4])=[O:2])=[C:13]2[N:8]([C:7]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH:9]=[CH:10][CH:11]=[CH:12]2

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 677721232-(3-Fluoro-2-methyl-benzyl)-3-phenyl-indolizine-1-carboxylic acid methyl ester

生成物 1

HCID 677747302-(3-Fluoro-2-methyl-benzyl)-3-phenyl-indolizine-1-carboxylic acid収率 107.1%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
90 °C

実験手順

The compound of step 3 (250 mg, 0.67 mmol) was dissolved in dioxane (10 ml) and treated with 10 ml of an aqueous 10 N solution of sodium hydroxide. The mixture was heated to 90° C. for 12 h, cooled to room temperature and neutralized with dilute hydrochloric acid. The aqueous phase was extracted with DCM and the combined organic phases dried over sodium sulfate and filtered. The solution was evaporated to give 258 mg of the crude title compound which was used in the next step without purification.

後処理

  1. extractionThe aqueous phase was extracted with DCM
  2. dry with materialthe combined organic phases dried over sodium sulfate
  3. filtrationfiltered
  4. customThe solution was evaporated

出典と根拠

ORDレコード
ord-282d5eabf8f34b50a4713a5a2e1d6c4d
出典データセット
uspto-grants-2013_04
特許番号
US08415336B2

反応ノート

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