Water → 10,11-dihydro-10,10,11,11tetrafluoro-5H-dibenzo[a,d]cyclohepten-5-ol

HRID 329232노트

반응식

HRID 329232 반응식
[BH4-].[Na+].O.[F:4][C:5]1([F:23])[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[C:9](=[O:16])[C:8]2[CH:17]=[CH:18][CH:19]=[CH:20][C:7]=2[C:6]1([F:22])[F:21]>C(O)(C)C>[F:4][C:5]1([F:23])[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[CH:9]([OH:16])[C:8]2[CH:17]=[CH:18][CH:19]=[CH:20][C:7]=2[C:6]1([F:21])[F:22]

참가 물질

5

반응물 3

HCID 962WaterHCID 4311764Sodium borohydrideHCID 2037337610,11-dihydro-10,10,11,11-tetrafluoro-5H-dibenzo[a,d]cyclohepten-5-one

생성물 1

HCID 2037337210,11-dihydro-10,10,11,11tetrafluoro-5H-dibenzo[a,d]cyclohepten-5-ol

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A solution of 190 mg. (0.005 mole) of sodium borohydride in 1 ml. of water is added dropwise to a stirred solution of 830 mg. (0.00296 mole) of 10,11-dihydro-10,10,11,11-tetrafluoro-5H-dibenzo[a,d]cyclohepten-5-one in 10 ml. of isopropyl alcohol. After stirring the mixture for 3 hours at room temperature and 30 minutes at reflux, the isopropyl alcohol is evaporated under reduced pressure. The residue is partitioned between benzene and water and the benzene extract is separated, washed, and dried. Evaporation under reduced pressure leaves the product as the residual pale yellow oil. A sample for analysis is evaporatively distilled at 80° C. and 0.1 mm.

후처리

  1. temperature30 minutes at reflux
  2. customthe isopropyl alcohol is evaporated under reduced pressure
  3. customThe residue is partitioned between benzene and water
  4. extractionthe benzene extract
  5. customis separated
  6. washwashed
  7. customdried
  8. customEvaporation under reduced pressure
  9. customleaves the product as the residual pale yellow oil
  10. distillationA sample for analysis is evaporatively distilled at 80° C.

출처 및 근거

ORD 기록
ord-bc02d1c2e7e54952bd30f939b825b823
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04020096

반응 노트

불러오는 중…