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Chloroform → 4-Hydroxy-7-iodoisoindolinone

HRID 21087
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HRID 21087 반응식
COC[O:4][C:5]1[CH:13]=[CH:12][C:11]([I:14])=[C:10]2[C:6]=1[CH2:7][N:8](C(C)(C1C=CC=CC=1)C)[C:9]2=[O:15].C(Cl)(Cl)Cl>Cl.CO>[OH:4][C:5]1[CH:13]=[CH:12][C:11]([I:14])=[C:10]2[C:6]=1[CH2:7][NH:8][C:9]2=[O:15]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6212ChloroformHCID 68490938HCID 68490938, 화합물

생성물 1

HCID 684897404-Hydroxy-7-iodoisoindolinone수율 85.1%

시약·촉매·용매 1

HCID 21893726Hydrochloride methanol용매2회

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온도
70 °C

실험 절차

4-Methoxymethoxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone (463 mg, 1.06 mmol) was dissolved in 10% hydrogen chloride-methanol solution (14 mL), and the solution was stirred at 70° C. for 2.5 hours. Then, the solution was added with 10% hydrogen chloride-methanol solution (4.3 mL) and further stirred at 2.5 hours. The reaction mixture was added with chloroform and purified by slurry. The solid was collected by filtration and washed with chloroform/methanol (9/1). The obtained solid was dried under reduced pressure to obtain 4-hydroxy-7-iodoisoindolinone (248 mg, yield 85%).

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후처리

  1. stirringfurther stirred at 2.5 hours
  2. custompurified by slurry
  3. filtrationThe solid was collected by filtration
  4. washwashed with chloroform/methanol (9/1)
  5. customThe obtained solid was dried under reduced pressure

출처 및 근거

ORD 기록
ord-909e71bd33ed45648f3d27ffa574164a
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07745641B2

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