Triethylamine → HCID 21306993, 화합물

HRID 29753

반응식

HRID 29753 반응식
[C:1]([O:5][C:6](=[O:16])[NH:7][C:8]1[CH:13]=[C:12]([CH2:14][OH:15])[CH:11]=[CH:10][N:9]=1)([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C>CS(C)=O>[C:1]([O:5][C:6](=[O:16])[NH:7][C:8]1[CH:13]=[C:12]([CH:14]=[O:15])[CH:11]=[CH:10][N:9]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

4

반응물 2

HCID 8471TriethylamineHCID 231510012-(Boc-amino)-4-(hydroxymethyl)pyridine

생성물 1

HCID 21306993HCID 21306993, 화합물수율 83%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

(4-Hydroxymethyl-pyridin-2-yl)-carbamic acid tert-butyl ester (1.91 g, 8.51 mmol) was dissolved in dry DMSO (10 mL) and the reaction flask immersed in a waterbath at 15° C. Triethylamine (1.72 g, 17.0 mmol) was added followed by sulfur trioxide pyridine complex (2.41 g, 15.1 mmol). The reaction mixture was stirred for 2 h and poured onto crushed ice and the product extracted with CHCl3. The organic extract was washed with water, dried concentrated under reduced pressure. The crude product was purified by flash chromatography (hexane/EtOAc, 80:20) to give (4-Formyl-pyridin-2-yl)-carbamic acid tert-butyl ester (1.57 g, 83%).

후처리

  1. customimmersed in a waterbath at 15° C
  2. additionpoured
  3. customonto crushed ice
  4. extractionthe product extracted with CHCl3
  5. extractionThe organic extract
  6. washwas washed with water
  7. customdried
  8. concentrationconcentrated under reduced pressure
  9. customThe crude product was purified by flash chromatography (hexane/EtOAc, 80:20)

출처 및 근거

ORD 기록
ord-42f7346519a941639e7046248c9023f6
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07423012B2

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