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Hydrochloric Acid → HCID 18477116, 화합물

HRID 2188200
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HRID 2188200 반응식
[CH2:1]([CH2:8][NH2:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:10].[F:11][C:12]1[CH:13]=[C:14]2[C:19](=[CH:20][CH:21]=1)[C:18](=[O:22])[CH2:17][CH2:16][CH2:15]2.[CH2:23]=O>C(O)C>[ClH:10].[CH2:1]([CH2:8][NH:9][CH2:23][CH:17]1[CH2:16][CH2:15][C:14]2[C:19](=[CH:20][CH:21]=[C:12]([F:11])[CH:13]=2)[C:18]1=[O:22])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 1001PhenethylamineHCID 149151166-Fluoro-1,2,3,4-tetrahydronaphthalen-1-one

생성물 1

HCID 18477116HCID 18477116, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To an ice-cooled solution of N-benzylmethylamine (5.67 cm3) in ethyl alcohol (60 cm3) was added hydrochloric acid (5 M, 10 cm3). 6-Fluoro-3,4-dihydro-2H-naphthalene-1-one (6.00 g) and paraformaldehyde (1.32 g) were then added and the resulting mixture was stirred and heated to reflux for 4 h. Upon cooling, the alcohol was removed under reduced pressure and water (100 cm3) was added. The remaining tetralone was extracted into diethyl ether (100 cm3) and the aqueous mixture was then extracted further with dichloromethane (2×100 cm3). The combined extracts were dried (Na2SO4) and concentrated under reduced pressure. Trituration with diethyl ether and filtration provided the title compound (3.18 g) as a white solid.

후처리

  1. temperatureheated
  2. temperatureto reflux for 4 h
  3. temperatureUpon cooling
  4. customthe alcohol was removed under reduced pressure and water (100 cm3)
  5. additionwas added
  6. extractionThe remaining tetralone was extracted into diethyl ether (100 cm3)
  7. extractionthe aqueous mixture was then extracted further with dichloromethane (2×100 cm3)
  8. dry with materialThe combined extracts were dried (Na2SO4)
  9. concentrationconcentrated under reduced pressure
  10. filtrationTrituration with diethyl ether and filtration

출처 및 근거

ORD 기록
ord-bbb8987766284a5284f65f81e84bdf78
출처 데이터셋
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06410592B1

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