HCID 178454124、化合物 → HCID 178454110、化合物

HRID 707264ノート

反応式

HRID 707264 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 99.2%

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

A mixture of tert-butyl(cis-3-azidocyclobutyl)carbamate (7.0 g, 33.0 mmol) and palladium 10% on activated carbon (3.51 ml, 33.0 mmol) in a three necked 1000 mL flask was flushed with nitrogen 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 at room temperature for 18 h, filtered, and the filtrate was evaporated under reduced pressure to give the desired product tert-butyl(cis-3-aminocyclobutyl)carbamate (6.1 g, 99% yield). 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 4.64 (br. s., 1 H), 3.72 (d, J=6.85 Hz, 1 H), 3.12 (t, J=7.73 Hz, 1 H), 2.71 (d, J=7.24 Hz, 2 H), 1.51 (q, J=9.85 Hz, 2 H), 1.43 (br. s., 11 H).

後処理

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

出典と根拠

ORDレコード
ord-adeca629a6e6467e85bb920ba0798b5e
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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