Acetone → 1-[(3-Methylpyridin-2-yl)oxy]-3-[(propan-2-yl)amino]propan-2-ol

HRID 647980노트

반응식

HRID 647980 반응식
Cl.[NH2:2][CH2:3][CH:4]([OH:14])[CH2:5][O:6][C:7]1[C:12]([CH3:13])=[CH:11][CH:10]=[CH:9][N:8]=1.C([BH3-])#N.[Na+].[CH3:19][C:20]([CH3:22])=O>CO>[OH:14][CH:4]([CH2:3][NH:2][CH:20]([CH3:22])[CH3:19])[CH2:5][O:6][C:7]1[C:12]([CH3:13])=[CH:11][CH:10]=[CH:9][N:8]=1

참가 물질

6

반응물 4

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 5003444Sodium cyanoborohydrideHCID 204835331-Amino-3-[(3-methylpyridin-2-yl)oxy]propan-2-ol

생성물 1

HCID 204835171-[(3-Methylpyridin-2-yl)oxy]-3-[(propan-2-yl)amino]propan-2-ol

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

4 ml of a 2 N solution of hydrogen chloride in methanol are added to a solution of 3.6 g of 2-(3'-amino-2'-hydroxy-propoxy)-3-methyl-pyridine and 1.5 g of sodium cyanoborohydride in 70 ml of methanol and 12 ml of acetone are added dropwise over the course of approx. 30 minutes, whilst stirring. The reaction mixture is stirred overnight at room temperature and is then evaporated in vacuo and the residue is acidified with 2 N hydrochloric acid. The aqueous solution is extracted once by shaking with 30 ml of ether. The hydrochloric acid phase is separated off and rendered alkaline with concentrated sodium hydroxide solution. 2-(2'-Hydroxy-3'-isopropylamino-propoxy)-3-methyl-pyridine is isolated by extraction with ethyl acetate and is identical with the material described in Example 21.

후처리

  1. additionare added dropwise over the course of approx. 30 minutes
  2. stirringThe reaction mixture is stirred overnight at room temperature
  3. customis then evaporated in vacuo
  4. extractionThe aqueous solution is extracted once
  5. stirringby shaking with 30 ml of ether
  6. customThe hydrochloric acid phase is separated off

출처 및 근거

ORD 기록
ord-63e5f333eae64bbbaf72137874d4965e
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04410530

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