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Hydrochloric Acid → 2-(4-Chlorophenyl)-2-(2,6-dichloro-4-nitrophenyl)acetonitrile

HRID 868303
ノート
印刷プレビュー

反応式

HRID 868303 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[C:4]([Cl:11])[C:3]=1Cl.[OH-].[Na+].[Cl:15][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][C:23]#[N:24])=[CH:18][CH:17]=1.Cl>[Cl-].C([N+](CC)(CC)CC1C=CC=CC=1)C.O1CCCC1>[Cl:11][C:4]1[CH:5]=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=[C:2]([Cl:1])[C:3]=1[CH:22]([C:19]1[CH:20]=[CH:21][C:16]([Cl:15])=[CH:17][CH:18]=1)[C:23]#[N:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 883653,4,5-TrichloronitrobenzeneHCID 2415824-Chlorobenzyl cyanide

生成物 1

HCID 150529152-(4-Chlorophenyl)-2-(2,6-dichloro-4-nitrophenyl)acetonitrile収率 93.3%

試薬・触媒・溶媒 2

HCID 66133
Benzyl triethylammonium chloride
触媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a stirred mixture of 45.3 parts of 1,2,3-trichloro-5-nitrobenzene, 300 parts of a sodium hydroxide solution 50%, 5 parts of N,N,N-triethylbenzenemethanaminium chloride and 360 parts of tetrahydrofuran was added dropwise, during a 5 minute period, a solution of 33.3 parts of 4-chlorobenzeneacetonitrile in 90 parts of tetrahydrofuran. Upon completion, stirring was continued for 4 hours at 50° C. The reaction mixture was poured into 1500 parts of crushed ice and acidified with concentrate hydrochloric acid. The product was extracted with trichloromethane. The extract was dried, filtered and evaporated. The residue was stirred in 2,2'-oxybispropane. The product was filtered off and dried, yielding 63.8 parts (93.3%) of 2,6-dichloro-α-(4-chlorophenyl)-4-nitrobenzeneacetonitrile (intermediate 3).

後処理

  1. additionwas added dropwise, during a 5 minute period
  2. additionThe reaction mixture was poured into 1500 parts of crushed ice
  3. extractionThe product was extracted with trichloromethane
  4. customThe extract was dried
  5. filtrationfiltered
  6. customevaporated
  7. stirringThe residue was stirred in 2,2'-oxybispropane
  8. filtrationThe product was filtered off
  9. customdried

出典と根拠

ORDレコード
ord-117d25d03b7e4a3787c11890557f93bc
出典データセット
uspto-grants-1988_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04778887

反応ノート

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