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Hydrochloric Acid → 6-Iodo-5-oxo-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-1-ylmethanol

HRID 132995
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HRID 132995 반응식
C([O:4][CH2:5][C:6]1[C:16]2[CH2:15][CH2:14][C:13]3[CH:17]=[CH:18][CH:19]=[C:20]([I:21])[C:12]=3[C:11](=[O:22])[C:10]=2[CH:9]=[CH:8][CH:7]=1)(=O)C.C(OCC1C2CCC3C=CC=CC=3C(=O)C=2C(I)=CC=1)(=O)C.O.Cl>O1CCCC1.CO.[OH-].[Na+]>[I:21][C:20]1[C:12]2[C:11](=[O:22])[C:10]3[CH:9]=[CH:8][CH:7]=[C:6]([CH2:5][OH:4])[C:16]=3[CH2:15][CH2:14][C:13]=2[CH:17]=[CH:18][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 12150903(6-iodo-5-oxo-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-1-yl)methyl acetateHCID 12150904(4-Iodo-5-oxo-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-1-yl)methyl acetate

생성물 1

HCID 586468506-Iodo-5-oxo-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-1-ylmethanol

시약·촉매·용매 3

HCID 887
Methanol
용매
HCID 8028Tetrahydrofuran용매
HCID 14798Sodium Hydroxide용매

실험 절차

1.5 g of the mixture of (6-iodo-5-oxo-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-1-yl)methyl acetate and (4-iodo-5-oxo-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-1-yl)methyl acetate prepared in Example 1-g was dissolved in a mixed solvent of 5 ml of tetrahydrofuran and 5 ml of methanol, and 0.1 ml of 5N sodium hydroxide solution was added at room temperature, followed by stirring at room temperature for 30 minutes. Water was added to the reaction mixture, and the mixture was neutralized with 5N hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and the solvent was evaporated, to give 1.3 g of a mixture of the title compound with a 4-iodo form as a colorless powder.

후처리

  1. additionwas added at room temperature
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-0bca8ded1dd44dc7837963c396463a27
출처 데이터셋
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07390797B2

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