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

HRID 2212256노트

반응식

HRID 2212256 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5dcb4d9fe1744e8aaf37e8585ad4c161
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07101905B2

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