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

HRID 132995
ノート
印刷プレビュー

反応式

HRID 132995 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 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

生成物 1

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

試薬・触媒・溶媒 3

HCID 887
Methanol
溶媒
HCID 8028Tetrahydrofuran溶媒
HCID 14798Sodium Hydroxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0bca8ded1dd44dc7837963c396463a27
出典データセット
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07390797B2

反応ノート

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