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

HRID 2268494노트

반응식

HRID 2268494 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e85350e1f35645c7b581a0e872feca04
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06326369B1

반응 노트

불러오는 중…