Sodium Hydroxide → HCID 13655355、化合物

HRID 745271ノート

反応式

HRID 745271 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH2:9][C:10]#[N:11].[OH-].[Na+].Br[CH2:15][CH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1>CN(C)C=O>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH:9]([CH2:15][CH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1)[C:10]#[N:11]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 805662,4-DichlorophenylacetonitrileHCID 137636Cyclohexane, (bromomethyl)-

生成物 1

HCID 13655355HCID 13655355、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 18.5 parts of 2,4-dichlorobenzeneacetonitrile and 180 parts of N,N-dimethylformamide is stirred and cooled in an ice-bath while nitrogen gas is introduced. 3.2 Parts of a sodium hydroxide solution 78% are added portionwise and the whole is stirred for one hour. Then there are added dropwise, during a one hour-period, 17.8 parts of (bromomethyl)cyclohexane while still cooling and while nitrogen gas is still introduced. Upon completion, stirring is continued for 2 hours at room temperature. The reaction mixture is poured onto water. The precipitated product is filtered off and triturated in a mixture of methanol and water. The product is filtered off and dried, yielding 25.5 parts of 2,4-dichloro-α-(cyclohexylmethyl)benzeneacetonitrile; mp. 58.8° C.

後処理

  1. temperaturecooled in an ice-bath while nitrogen gas
  2. additionis introduced
  3. stirringthe whole is stirred for one hour
  4. temperaturewhile still cooling and while nitrogen gas
  5. additionis still introduced
  6. stirringUpon completion, stirring
  7. additionThe reaction mixture is poured onto water
  8. filtrationThe precipitated product is filtered off
  9. customtriturated in a mixture of methanol and water
  10. filtrationThe product is filtered off
  11. customdried

出典と根拠

ORDレコード
ord-c2d8cbe2136342b0b26a3ce2167930ec
出典データセット
uspto-grants-1986_07
特許番号
US04598085

反応ノート

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