Ammonium Chloride → HCID 57832734, 화합물

HRID 729454노트

반응식

HRID 729454 반응식
[Br:1][C:2]1[CH:22]=[CH:21][C:20]([F:23])=[CH:19][C:3]=1[O:4][CH:5]1[CH2:10][CH2:9][N:8]([C:11]2[N:12]=[CH:13][C:14]([C:17]#[N:18])=[N:15][CH:16]=2)[CH2:7][CH2:6]1.[N-:24]=[N+:25]=[N-:26].[Na+].[Cl-].[NH4+]>CN(C=O)C>[Br:1][C:2]1[CH:22]=[CH:21][C:20]([F:23])=[CH:19][C:3]=1[O:4][CH:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[N:15][C:14]([C:17]3[N:24]=[N:25][NH:26][N:18]=3)=[CH:13][N:12]=2)[CH2:7][CH2:6]1

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 688192205-[4-(2-Bromo-5-fluorophenoxy)piperidin-1-yl]pyrazine-2-carbonitrile

생성물 1

HCID 57832734HCID 57832734, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 5-[4-(2-bromo-5-fluorophenoxy)piperidin-1-yl]pyrazine-2-carbonitrile from Step 5 (0.200 g, 0.530 mmol) in DMF (2 mL) was added sodium azide (0.070 g, 1.06 mmol) and ammonium chloride (0.284 g, 5.30 mmol). After a period of 3 h at 130° C., the reaction mixture was cooled and partitioned between ethyl acetate and brine. The organic phase was separated, dried over sodium sulfate and evaporated. To the crude product was added a mixture of ether-hexane (1:1). The resulting solid was filtered to provide the title compound.

후처리

  1. temperaturethe reaction mixture was cooled
  2. custompartitioned between ethyl acetate and brine
  3. customThe organic phase was separated
  4. dry with materialdried over sodium sulfate
  5. customevaporated
  6. additionTo the crude product was added
  7. additiona mixture of ether-hexane (1:1)
  8. filtrationThe resulting solid was filtered

출처 및 근거

ORD 기록
ord-a359bc09b15043a59a73a17b106b7778
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07582633B2

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