Sodium hydride → HCID 13149080, 화합물

HRID 1613608노트

반응식

HRID 1613608 반응식
[H-].[Na+].Br[C@H:4]1[C@H:10]([OH:11])[C:9]2[CH:12]=[CH:13][CH:14]=[CH:15][C:8]=2[O:7][CH2:6][CH2:5]1>CS(C)=O>[O:11]1[CH:10]2[CH:4]1[CH2:5][CH2:6][O:7][C:8]1[CH:15]=[CH:14][CH:13]=[CH:12][C:9]=12

참가 물질

4

반응물 2

HCID 24758Sodium hydrideHCID 13149516HCID 13149516, 화합물

생성물 1

HCID 13149080HCID 13149080, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매2회

실험 절차

8.60 g (0.298 mole) of sodium hydride (80% dispersion in mineral oil) are introduced under argon into 320 ml of DMSO, and a solution of 243 g (0.259 mole) of trans-4-bromo-5-hydroxy-2,3,4,5-tetrahydro-1-benzoxepin in 180 ml of DMSO is added dropwise at room temperature within 2.5 hours. After 3 hours, the mixture is poured onto ice/water with stirring, and is extracted 3 times with diethyl ether. The combined organic phases are washed with water and saturated sodium chloride solution, dried over sodium sulfate and filtered, and the solvent is evaporated off in vacuo. The remaining 44 g of oil is distilled at 67°-69° C./0.01 torr.

후처리

  1. additionthe mixture is poured onto ice/water
  2. extractionis extracted 3 times with diethyl ether
  3. washThe combined organic phases are washed with water and saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customthe solvent is evaporated off in vacuo
  7. distillationThe remaining 44 g of oil is distilled at 67°-69° C./0.01 torr

출처 및 근거

ORD 기록
ord-97c69892c95e4fec95e18d0f293978fb
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05194442

반응 노트

불러오는 중…