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Water → HCID 22396212, 화합물

HRID 1070494
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HRID 1070494 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[N:11]=[C:10]([CH2:12][CH2:13][C:14]([OH:16])=O)[O:9][N:8]=1.Cl.[NH2:18][CH:19]1[CH2:24][CH2:23][N:22]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:21][CH2:20]1.C(N(CC)CC)C.O>ClCCl.[Cl-].[Na+].O>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[N:11]=[C:10]([CH2:12][CH2:13][C:14]([NH:18][CH:19]2[CH2:20][CH2:21][N:22]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:23][CH2:24]2)=[O:16])[O:9][N:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 2756033tert-Butyl 4-aminopiperidine-1-carboxylate--hydrogen chloride (1/1)HCID 31643283-(3-(Pyridin-2-yl)-1,2,4-oxadiazol-5-yl)propanoic acid

생성물 1

HCID 22396212HCID 22396212, 화합물수율 47.2%

시약·촉매·용매 2

HCID 6344
Dichloromethane
용매
2회
HCID 57417360Sodium chloride; water용매

실험 절차

3-[3-(2-Pyridinyl)-1,2,4-oxadiazol-5-yl]propanoic acid (0.60 g) was dissolved in dichloromethane (10 ml). 1,1-Carbonyldiimidazole (0.33 g) was added followed by tert-butyl 4-amino-1-piperidinecarboxylate hydrochloride (0.5 g) and triethylamine (0.31 ml). After 2 hours water, brine and dichloromethane were added and the phases separated. The organic phase was dried, filtered and evaporated and the residue was purified by chromatography eluting with ethyl acetate:methanol (33:1) to give the subtitle compound (0.40 g).

후처리

  1. customthe phases separated
  2. customThe organic phase was dried
  3. filtrationfiltered
  4. customevaporated
  5. customthe residue was purified by chromatography
  6. washeluting with ethyl acetate:methanol (33:1)

출처 및 근거

ORD 기록
ord-c630edc8876343cd9980609724eae112
출처 데이터셋
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06903085B1

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