Dimethylamine, hydrochloride → HCID 22278842, 화합물

HRID 746862노트

반응식

HRID 746862 반응식
C([BH3-])#N.[Na+].C(OC([N:12]1[CH2:17][CH2:16][C:15](=O)[CH:14]([CH2:19][CH3:20])[CH2:13]1)=O)(C)(C)C.Cl.[CH3:22][NH:23][CH3:24].[OH-].[K+]>CO>[CH3:22][N:23]([CH3:24])[CH:15]1[CH2:16][CH2:17][NH:12][CH2:13][CH:14]1[CH2:19][CH3:20]

참가 물질

6

반응물 4

HCID 10473Dimethylamine, hydrochlorideHCID 14797Potassium HydroxideHCID 5003444Sodium cyanoborohydrideHCID 22278903tert-Butyl 3-ethyl-4-oxopiperidine-1-carboxylate

생성물 1

HCID 22278842HCID 22278842, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Sodium cyanoborohydride (3.2 g, 50.8 mmol) was added to the stirred suspension of N-tert.-butoxycarbonyl-3-ethyl-4-piperidone (8 g, 35 mmol), N,N-dimethylamine hydrochloride (14 g, 172 mmol) and KOH (9.6 g, 172 mmol) in methanol (50 ml) at 0° C. The resulting mixture was stirred for 4 hr at ambient temperature. The reaction mixture was concentrated to dryness, triturated with water, acidified with conc. HCl (pH 3˜4) and extracted with ethyl acetate to remove impurities. The aqueous layer was basified with 1 M sodium hydroxide solution (pH ˜10) and extracted with ethyl acetate. Ethyl acetate extract was dried (Na2SO4) and concentrated to dryness to give 4-dimethylamino-3-ethylpiperidine. Yield 2.3 g (37%), C9H20N2, m/z 157 (M+1).

후처리

  1. concentrationThe reaction mixture was concentrated to dryness
  2. customtriturated with water
  3. extractionextracted with ethyl acetate
  4. customto remove impurities
  5. extractionextracted with ethyl acetate
  6. extractionEthyl acetate extract
  7. dry with materialwas dried (Na2SO4)
  8. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-0f683f81cf70488087a8661dc530b58b
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07393957B2

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