Ethyl Acetate → 4-(2H-1,2,3,4-tetrazol-2-yl)aniline

HRID 1798822

반응식

HRID 1798822 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]2[N:14]=[N:13][CH:12]=[N:11]2)=[CH:6][CH:5]=1)([O-])=O.C(OCC)(=O)C>C(O)C.[Pd]>[N:11]1[N:10]([C:7]2[CH:8]=[CH:9][C:4]([NH2:1])=[CH:5][CH:6]=2)[N:14]=[N:13][CH:12]=1

참가 물질

5

반응물 2

HCID 8857Ethyl AcetateHCID 5338832-(4-Nitrophenyl)-2H-tetrazole

생성물 1

HCID 5716394-(2H-1,2,3,4-tetrazol-2-yl)aniline

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

2-(4-Nitrophenyl)-2H-tetrazole (200 mg, 1.05 mmol) was suspended in ethanol (1 mL). Ethyl acetate (1 mL) was added to improved solubility. The solution was degassed and purged with nitrogen 3 times before palladium on carbon (10% w/w, 223 mg, 0.2 mmol) was added. The mixture was degassed and purged with hydrogen 3 times and stirred under a hydrogen balloon for 2 hours. The reaction was diluted with acetone and passed through a plug of silica gel, which was washed thoroughly with acetone. The filtrated was concentrated to give the crude product which was used as isolated.

후처리

  1. customThe solution was degassed
  2. additionwas added
  3. customThe mixture was degassed
  4. custompurged with hydrogen 3 times
  5. additionThe reaction was diluted with acetone
  6. washwas washed thoroughly with acetone
  7. concentrationThe filtrated was concentrated

출처 및 근거

ORD 기록
ord-bd431c95bcb042a0809cfc1f3f247942
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08343990B2

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