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

HRID 1483028ノート

反応式

HRID 1483028 の反応式
[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

参加物

4

反応物 1

HCID 90134886HCID 90134886、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-40bcf2a8a5cd40ac9b7b21c8885c8398
出典データセット
uspto-grants-2016_08
特許番号
US09416138B2

反応ノート

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