HCID 178454124, 화합물 → HCID 178454110, 화합물

HRID 707425노트

반응식

HRID 707425 반응식
[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]

참가 물질

3

반응물 1

HCID 178454124HCID 178454124, 화합물

생성물 1

HCID 178454110HCID 178454110, 화합물수율 84.3%

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0aaa1f83639240048bd3ae9ccf498850
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09174992B2

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