Benzylamine → HCID 69256693, 화합물

HRID 1793339노트

반응식

HRID 1793339 반응식
CS(O[CH2:6][C@H:7]1[O:16][C:11]2=[N:12][CH:13]=[CH:14][CH:15]=[C:10]2[O:9][CH2:8]1)(=O)=O.[CH2:17]([NH2:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C([O-])(O)=O.[Na+]>O1CCOCC1>[C:18]1([CH2:17][NH:24][CH2:6][C@@H:7]2[O:16][C:11]3=[N:12][CH:13]=[CH:14][CH:15]=[C:10]3[O:9][CH2:8]2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

참가 물질

5

반응물 3

HCID 7504BenzylamineHCID 516892Sodium BicarbonateHCID 131725870HCID 131725870, 화합물

생성물 1

HCID 69256693HCID 69256693, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of intermediate (3) (0.041 mol), benzylamine (0.041 mol) and NaHCO3 (0.11 mol) in dioxane (100 ml) was stirred and refluxed for 48 hours. The solvent was evaporated. The residue was taken up in water and DCM. The separated organic layer was dried, filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5). The desired fractions were collected, the solvent was evaporated, yielding (S)-2,3-dihydro-N-(phenylmethyl)-[1,4]dioxino[2,3-b]pyridine-3-methanamine (intermediate 55).

후처리

  1. temperaturerefluxed for 48 hours
  2. customThe solvent was evaporated
  3. customThe separated organic layer was dried
  4. filtrationfiltered
  5. customthe solvent was evaporated
  6. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5)
  7. customThe desired fractions were collected
  8. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-5e097a300e7d4722996dea0fb55be713
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07081453B2

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