HCID 178454124、化合物 → HCID 178454110、化合物

HRID 707425ノート

反応式

HRID 707425 の反応式
[C:1]([O:5][C:6](=[O:15])[NH:7][C@H:8]1[CH2:11][C@@H:10]([N:12]=[N+]=[N-])[CH2:9]1)([CH3:4])([CH3:3])[CH3:2]>[Pd]>[C:1]([O:5][C:6](=[O:15])[NH:7][C@H:8]1[CH2:11][C@@H:10]([NH2:12])[CH2:9]1)([CH3:4])([CH3:2])[CH3:3]

参加物

3

反応物 1

HCID 178454124HCID 178454124、化合物

生成物 1

HCID 178454110HCID 178454110、化合物収率 84.3%

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

A mixture of tert-butyl(cis-3-azidocyclobutyl)carbamate (15.00 g, 70.7 mmol) and palladium 10 wt. % (dry basis) on activated carbon, wet (3.76 ml, 35.3 mmol, Sigma-Aldrich Chemical Company, Inc.) in three necked 1000 mL flask was flushed with N2 and closed tightly and 2M ammonia in methanol solution (200 mL) was added. The flask was evacuated and a balloon filled with hydrogen was introduced. The mixture was stirred for 18 h, filtered, and the filtrate was evaporated under reduced pressure to give the title compound (11.1 g, 59.6 mmol, 84% yield), which was used in the next step without further purification.

後処理

  1. customwas flushed with N2
  2. customclosed tightly
  3. addition2M ammonia in methanol solution (200 mL) was added
  4. customThe flask was evacuated
  5. additiona balloon filled with hydrogen
  6. additionwas introduced
  7. filtrationfiltered
  8. customthe filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-0aaa1f83639240048bd3ae9ccf498850
出典データセット
uspto-grants-2015_11
特許番号
US09174992B2

反応ノート

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