Ammonium Chloride → HCID 57832734、化合物

HRID 729454ノート

反応式

HRID 729454 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 57832734HCID 57832734、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a359bc09b15043a59a73a17b106b7778
出典データセット
uspto-grants-2009_09
特許番号
US07582633B2

反応ノート

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