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Hydrochloric Acid → HCID 178423539, 화합물

HRID 417143
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HRID 417143 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([CH:13]([CH:26]3[CH2:31][CH2:30][C:29]([F:33])([F:32])[CH2:28][CH2:27]3)[CH2:14][O:15][C:16]3[C:23]([CH3:24])=[CH:22][C:19]([C:20]#[N:21])=[CH:18][C:17]=3[CH3:25])[C:11]3[CH:34]=[C:35]([F:39])[C:36]([F:38])=[CH:37][C:10]=3[N:9]=2)=[CH:4][CH:3]=1.Cl.C(N(CC)CC)C.[N-:48]=[N+:49]=[N-:50].[Na+].Cl>CC1C=CC=CC=1C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([CH:13]([CH:26]3[CH2:27][CH2:28][C:29]([F:33])([F:32])[CH2:30][CH2:31]3)[CH2:14][O:15][C:16]3[C:23]([CH3:24])=[CH:22][C:19]([C:20]4[NH:50][N:49]=[N:48][N:21]=4)=[CH:18][C:17]=3[CH3:25])[C:11]3[CH:34]=[C:35]([F:39])[C:36]([F:38])=[CH:37][C:10]=3[N:9]=2)=[CH:4][CH:3]=1
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6

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HCID 313Hydrochloric AcidHCID 11130Triethylamine hydrochloride2회HCID 33557Sodium Azide2회HCID 666195364-[2-[2-(4-Chloro-phenyl)-5,6-difluoro-benzoimidazol-1-yl]-2-(4,4-difluoro-cyclohexyl)-ethoxy]-3,5-dimethyl-benzonitrile

생성물 1

HCID 178423539HCID 178423539, 화합물

시약·촉매·용매 1

HCID 7237
O-Xylene
용매

반응 조건

온도
150 °C

실험 절차

To a solution of 0.16 g (0.29 mmol) 4-[2-[2-(4-chloro-phenyl)-5,6-difluoro-benzoimidazol-1-yl]-2-(4,4-difluoro-cyclohexyl)-ethoxy]-3,5-dimethyl-benzonitrile in 4 ml o-xylene were added 0.198 g (1.44 mmol) triethylamine hydrochloride and 0.094 g (1.45 mmol) sodium azide and heated for 21 h at 150° C. (oil bath temperature). Another 0.198 g (1.44 mmol) triethylamine hydrochloride and 0.094 g (1.45 mmol) sodium azide were added and the reaction mixture was heated for another 4 h and after cooling down to room temperature stirred 3 days. The reaction was then poured onto 1M aqueous hydrochloric acid solution, the phases were separated and the aqueous phase extracted three times with ethyl acetate. The combined organic layers were washed with brine, dried over magnesium sulfate, filtered and evaporated. The solid was suspended in acetonitrile, filtered, washed with acetonitrile and dried under high vacuum. White solid (77%). MS (Turbo Spray): m/z=599.194 [M+H].

후처리

  1. temperaturethe reaction mixture was heated for another 4 h
  2. temperatureafter cooling down to room temperature
  3. customthe phases were separated
  4. extractionthe aqueous phase extracted three times with ethyl acetate
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. customevaporated
  9. filtrationfiltered
  10. washwashed with acetonitrile
  11. customdried under high vacuum

출처 및 근거

ORD 기록
ord-43749cc31f04477a8b38c2cc0b6ddd27
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08088930B2

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