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Hydrochloric Acid → HCID 86712401, 화합물

HRID 2174196
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HRID 2174196 반응식
[Br:1][C:2]1[C:3]([C:8]([CH3:12])([CH3:11])[C:9]#N)=[N:4][CH:5]=[CH:6][CH:7]=1.[H-].C([Al+]CC(C)C)C(C)C.Cl.C(=O)([O-])[OH:25].[Na+]>C1(C)C=CC=CC=1>[Br:1][C:2]1[C:3]([C:8]([CH3:12])([CH3:11])[CH:9]=[O:25])=[N:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 21225700Diisobutylaluminumhydride2회HCID 867123981415018-68-6

생성물 1

HCID 86712401HCID 86712401, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

1.8 g of 2-(3-bromo-pyridin-2-yl)-2-methyl-propionitrile were dissolved in 20 ml of toluene. 5.9 ml of a 25% by weight toluene solution of diisobutylaluminum hydride were added thereto at 0° C. The mixture was stirred for 17 hours at room temperature. Subsequently, dilute hydrochloric acid was added thereto to dissolve the unreacted diisobutylaluminum hydride. Continuing, aqueous saturated sodium hydrogen carbonate solution was added thereto followed by extracting with ethyl acetate. The solvent of the organic phase was distilled off followed by purifying by silica gel column chromatography to obtain 0.44 g of 2-(3-bromo-pyridin-2-yl)-2-methyl-propioaldehyde.

후처리

  1. customat 0° C
  2. extractionby extracting with ethyl acetate
  3. distillationThe solvent of the organic phase was distilled off
  4. customby purifying by silica gel column chromatography

출처 및 근거

ORD 기록
ord-5726306167bb45db90d7f12dd561f89f
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09060517B2

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