HCID 90134886, 화합물 → [(3S)-2,3-Dihydro-[1,4]dioxino[2,3-b]pyridin-3-yl]methanamine

HRID 1483028노트

반응식

HRID 1483028 반응식
[N:1]([CH2:4][C@@H:5]1[O:14][C:9]2=[N:10][CH:11]=[CH:12][CH:13]=[C:8]2[O:7][CH2:6]1)=[N+]=[N-]>CO.[Pd]>[O:7]1[C:8]2[C:9](=[N:10][CH:11]=[CH:12][CH:13]=2)[O:14][C@@H:5]([CH2:4][NH2:1])[CH2:6]1

참가 물질

4

반응물 1

HCID 90134886HCID 90134886, 화합물

생성물 1

HCID 68531823[(3S)-2,3-Dihydro-[1,4]dioxino[2,3-b]pyridin-3-yl]methanamine수율 100.2%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

Dissolve (3S)-3-(azidomethyl)-2,3-dihydro-[1,4]dioxino[2,3-b]pyridine (7.5 g, 39.03 mmol) in MeOH (390 mL). Degas the mixture by subjecting it to reduced pressure then back filling with nitrogen (3×); add 10% Pd/C (2.08 g, 1.95 mmol); and again degas the mixture. Stir the resulting degassed mixture at ambient temperature under a hydrogen atmosphere for 17 hours. Filter the resulting mixture through Celite® and remove solvents of the filtrate under reduced pressure to provide the title compound (6.5 g, 100%) as an oil. MS (m/z): 167 (M+1).

후처리

  1. customDegas the mixture
  2. customand again degas the mixture
  3. customdegassed mixture at ambient temperature under a hydrogen atmosphere for 17 hours
  4. filtrationFilter the resulting mixture through Celite®
  5. customremove solvents of the filtrate under reduced pressure

출처 및 근거

ORD 기록
ord-40bcf2a8a5cd40ac9b7b21c8885c8398
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09416138B2

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