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Hydrochloric Acid → HCID 11951932、化合物

HRID 1291697
ノート
印刷プレビュー

反応式

HRID 1291697 の反応式
[Cl:1][C:2]1[CH:9]=[CH:8][C:7]([C:10]([F:13])([F:12])[F:11])=[CH:6][C:3]=1[CH:4]=O.[CH3:14][NH2:15].S([O-])([O-])(=O)=O.[Mg+2].[BH4-].[Na+].Cl>C1COCC1.CO>[Cl:1][C:2]1[CH:9]=[CH:8][C:7]([C:10]([F:13])([F:12])[F:11])=[CH:6][C:3]=1[CH2:4][NH:15][CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 6329MethylamineHCID 24083Sulfuric acid magnesium salt (1:1)HCID 6881812-Chloro-5-(trifluoromethyl)benzaldehydeHCID 4311764Sodium borohydride

生成物 1

HCID 11951932HCID 11951932、化合物

試薬・触媒・溶媒 2

HCID 887
Methanol
溶媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

2.1 g of 2-chloro-5-trifluoromethylbenzaldehyde, 15 ml of methylamine and 2 g of magnesium sulfate were stirred at room temperature for 2 h, the excess methylamine for the most part evaporating. The reaction mixture was diluted with ether, filtered and concentrated in vacuo. The methylbenzimine thus obtained was dissolved in 15 ml of THF and added dropwise to a suspension of 1.5 g of sodium borohydride in 15 ml of THF. After stirring overnight, the mixture was treated with 30 ml of methanol, stirred for a further 30 min and then rendered acidic with dil. hydrochloric acid. It was extracted with tert-butyl methyl ether, and the aqueous phase was rendered alkaline and extracted twice again with tert-butyl methyl ether. After concentrating this extract, 1.0 g of N-(2-chloro-5-trifluoromethylbenzyl)-N-methylamine was obtained.

後処理

  1. customthe excess methylamine for the most part evaporating
  2. additionThe reaction mixture was diluted with ether
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe methylbenzimine thus obtained
  6. stirringstirred for a further 30 min
  7. extractionIt was extracted with tert-butyl methyl ether
  8. extractionextracted twice again with tert-butyl methyl ether
  9. concentrationAfter concentrating this extract

出典と根拠

ORDレコード
ord-56aa62ef91b84579b5dad93babe39437
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05753710

反応ノート

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