p-Toluenesulfonic acid monohydrate → HCID 178418333, 화합물

HRID 1403

반응식

HRID 1403 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]#[C:9][CH:10](O)[CH2:11][C@H:12]2[CH2:17][CH2:16][Si@H:15]([CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])[CH2:14][CH2:13]2)=[CH:4][CH:3]=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1C=CC=CC=1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]#[C:9]/[CH:10]=[CH:11]/[C@H:12]2[CH2:13][CH2:14][Si@H:15]([CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])[CH2:16][CH2:17]2)=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 178418481HCID 178418481, 화합물

생성물 1

HCID 178418333HCID 178418333, 화합물수율 15.9%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A mixture of 1-(4-fluorophenyl)-4-(trans-4-pentyl-4-silacyclohexyl)-1-butyne-3-ol 8.0 g (24 mmol), p-toluenesulfonic acid monohydrate 1.6 g, and benzene 200 ml was heated under reflux to remove the water and then subjected to a conventional post-treatment. The reaction mixture thus obtained was not only a mixture of trans- and cis-isomers, with respect to the silacyclohexane ring, but also a mixture of E- and Z-isomers, with respect to the double bond. Hence, the product was separated by chromatography to give 1.2 g of the desired product of the trans-E isomer (yield 15.9%).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux
  3. customto remove the water
  4. customThe reaction mixture thus obtained
  5. additiona mixture of trans- and cis-isomers
  6. additionwith respect to the silacyclohexane ring, but also a mixture of E- and Z-isomers
  7. customHence, the product was separated by chromatography

출처 및 근거

ORD 기록
ord-62dac6c13c4c4aa59ca7877a94095e3c
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05725797

연결된 노트

불러오는 중…