Hydrochloric Acid → 2-(1,3-Dioxo-1,3-dihydroisoindol-2-yl)-4-phenyl-thiophene-3-carboxylic acid

HRID 2212256ノート

反応式

HRID 2212256 の反応式
[OH-].[Na+].CO.C([O:7][C:8]([C:10]1[C:14]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[CH:13][S:12][C:11]=1[N:21]1[C:29](=[O:30])[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[C:22]1=[O:31])=[O:9])C.Cl>O>[O:30]=[C:29]1[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[C:22](=[O:31])[N:21]1[C:11]1[S:12][CH:13]=[C:14]([C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)[C:10]=1[C:8]([OH:9])=[O:7]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 70358872-(1,3-Dioxo-1,3-dihydroisoindol-2-yl)-4-phenyl-thiophene-3-carboxylic acid ethyl ester

生成物 1

HCID 219643732-(1,3-Dioxo-1,3-dihydroisoindol-2-yl)-4-phenyl-thiophene-3-carboxylic acid収率 92%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To a solution of NaOH (1.4 mmol) in a 1:1 mixture of methanol:H2O (6 mL) was added 2-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-4-phenyl-thiophene-3-carboxylic acid ethyl ester (0.7 mmol, Example 1, Part C). The mixture was heated to reflux for 90 minutes, then diluted with water (12 mL), chilled in an ice bath, and acidified with concentrated HCl. The product that precipitated was collected by filtration, washed with water, and dried, affording the desired compound as a white solid in 92% yield.

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 90 minutes
  3. temperaturechilled in an ice bath
  4. customThe product that precipitated
  5. filtrationwas collected by filtration
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-5dcb4d9fe1744e8aaf37e8585ad4c161
出典データセット
uspto-grants-2006_09
特許番号
US07101905B2

反応ノート

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