Acetone → 7-(2-Iodoethyl)-1,2,3,4-tetramethoxy-6,7,8,9-tetrahydro-5H-benzo[a]cycloheptene

HRID 2268494ノート

反応式

HRID 2268494 の反応式
CS(O[CH2:6][CH2:7][CH:8]1[CH2:14][CH2:13][C:12]2[C:15]([O:25][CH3:26])=[C:16]([O:23][CH3:24])[C:17]([O:21][CH3:22])=[C:18]([O:19][CH3:20])[C:11]=2[CH2:10][CH2:9]1)(=O)=O.[I-:27].[Na+].CC(C)=O>O>[I:27][CH2:6][CH2:7][CH:8]1[CH2:14][CH2:13][C:12]2[C:15]([O:25][CH3:26])=[C:16]([O:23][CH3:24])[C:17]([O:21][CH3:22])=[C:18]([O:19][CH3:20])[C:11]=2[CH2:10][CH2:9]1

参加物

5

反応物 3

HCID 180AcetoneHCID 5238Sodium IodideHCID 183485372-(1,2,3,4-tetramethoxy-6,7,8,9-tetrahydro-5H-benzo[a]cyclohepten-7-yl)ethyl methanesulfonate

生成物 1

HCID 183485187-(2-Iodoethyl)-1,2,3,4-tetramethoxy-6,7,8,9-tetrahydro-5H-benzo[a]cycloheptene収率 97.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The mixture of 2-(1,2,3,4-tetramethoxy-6,7,8,9-tetrahydro-5H-benzo[a]cyclohepten-7-yl)ethyl methanesulfonate (3.12 g), sodium iodide (3.61 g), and acetone (40 ml) was heated under reflux for 1 hr. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with 5% aqueous sodium sulfite, water, and saturated aqueous sodium chloride, and dried. The solvent was removed in vacuo to yield the entitled compound (3.29 g) as crystals.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 1 hr
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with 5% aqueous sodium sulfite, water, and saturated aqueous sodium chloride
  5. customdried
  6. customThe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-e85350e1f35645c7b581a0e872feca04
出典データセット
uspto-grants-2001_12
特許番号
US06326369B1

反応ノート

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