Tetrahydrofuran → HCID 11108683、化合物

HRID 440157ノート

反応式

HRID 440157 の反応式
O1CCCC1.[Cl:6][C:7]1[CH:13]=[C:12]([Cl:14])[C:11]([F:15])=[CH:10][C:8]=1[NH2:9].[F:16][B-:17]([F:20])([F:19])[F:18].[H+].[N:22]([O-])=O.[Na+]>O>[F:16][B-:17]([F:20])([F:19])[F:18].[Cl:6][C:7]1[CH:13]=[C:12]([Cl:14])[C:11]([F:15])=[CH:10][C:8]=1[N+:9]#[N:22]

参加物

6

反応物 4

HCID 8028TetrahydrofuranHCID 28118Tetrafluoroboric acidHCID 27580982,4-Dichloro-5-fluoroanilineHCID 23668193Sodium Nitrite

生成物 1

HCID 11108683HCID 11108683、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

165 ml of tetrahydrofuran are added to 100 g of 2,4-dichloro-5-fluoroaniline at room temperature. To this solution are added 333 ml of tetrafluoroboric acid (50% strength) with cooling. 57.5 g of sodium nitrite in 117 ml of water are added to the reaction mixture cooled to 5°-10° C. in such a way that the internal temperature is 7°-13° C. After addition is completed, the 0° C. solution is filtered. The residue is washed with tetrahydrofuran and ice-cold water. 121 g of product remain.

後処理

  1. temperaturewith cooling
  2. temperaturecooled to 5°-10° C. in such a way that the internal temperature
  3. customis 7°-13° C
  4. additionAfter addition
  5. filtrationthe 0° C. solution is filtered
  6. washThe residue is washed with tetrahydrofuran and ice-cold water

出典と根拠

ORDレコード
ord-75ccc428b7784551b3c69c9012b774d2
出典データセット
uspto-grants-1996_05
特許番号
US05516932

反応ノート

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