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Hydrochloric Acid → HCID 11951932, 화합물

HRID 376898
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HRID 376898 반응식
[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]
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반응물 5

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

생성물 1

HCID 11951932HCID 11951932, 화합물

시약·촉매·용매 2

HCID 887
Methanol
용매
HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-14f7924a83e74a80bd6f1ef440149a7d
출처 데이터셋
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06022899

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