3-Fluorophenylhydrazine hydrochloride → 7-Fluoro-N,N-dimethyl-2,3,4,9-tetrahydro-1H-carbazol-3-amine

HRID 128116

반응식

HRID 128116 반응식
Cl.[CH3:2][N:3]([CH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][C:6]1=O)[CH3:4].Cl.[F:13][C:14]1[CH:15]=[C:16]([NH:20]N)[CH:17]=[CH:18][CH:19]=1>C(O)C>[CH3:2][N:3]([CH3:4])[CH:5]1[CH2:10][C:9]2[C:17]3[C:16](=[CH:15][C:14]([F:13])=[CH:19][CH:18]=3)[NH:20][C:8]=2[CH2:7][CH2:6]1

참가 물질

4

반응물 2

HCID 27239143-Fluorophenylhydrazine hydrochlorideHCID 23470418Dimethylaminocyclohexanone hydrochloride

생성물 1

HCID 123618347-Fluoro-N,N-dimethyl-2,3,4,9-tetrahydro-1H-carbazol-3-amine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 35.5 g. of dimethylaminocyclohexanone hydrochloride and 34.5 g. of 3-fluorophenylhydrazine hydrochloride in 500 ml. of absolute ethyl alcohol was heated at reflux for twenty hours and then cooled in an ice bath. The resulting crystals were collected by filtration, suspended in chloroform, and treated with dilute potassium hydroxide. The chloroform layer was separated and evaporated to dryness under reduced pressure to give, after recrystallization from isopropyl alcohol, 31.5 g. of 3-(dimethylamino)-7-fluoro-1,2,3,4-tetrahydrocarbazole, m.p. 174°-176° C.

후처리

  1. temperatureat reflux for twenty hours
  2. temperaturecooled in an ice bath
  3. filtrationThe resulting crystals were collected by filtration
  4. additiontreated with dilute potassium hydroxide
  5. customThe chloroform layer was separated
  6. customevaporated to dryness under reduced pressure
  7. customto give
  8. customafter recrystallization from isopropyl alcohol, 31.5 g

출처 및 근거

ORD 기록
ord-35d4fee6b18443139088625895e15fa4
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04257952

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