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Ammonium formate → 2-Amino-1-[4-(methylthio)phenyl]ethanol

HRID 1908254
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HRID 1908254 반응식
[N:1]([CH2:4][CH:5]([C:7]1[CH:12]=[CH:11][C:10]([S:13][CH3:14])=[CH:9][CH:8]=1)[OH:6])=[N+]=[N-].C([O-])=O.[NH4+]>[Pd].CO>[NH2:1][CH2:4][CH:5]([C:7]1[CH:12]=[CH:11][C:10]([S:13][CH3:14])=[CH:9][CH:8]=1)[OH:6]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 2723923Ammonium formateHCID 86635142HCID 86635142, 화합물

생성물 1

HCID 167683402-Amino-1-[4-(methylthio)phenyl]ethanol수율 72%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

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온도
64 °C

실험 절차

To a stirred rt suspension consisting of 2-azido-1-(4-methylsulfanyl-phenyl)-ethanol (104.6 mg, 0.50 mmol), 10% Pd/C (100 mg, 0.10 mmol) and MeOH (25 mL) was added ammonium formate (316 mg, 5.0 mmol) under a N2 atmosphere. The resulting mixture was heated at 64° C. for 2 h. After cooling to rt, the catalyst was removed by filtration through a pad of celite and the celite pad washed with MeOH. The filtrate was concentrated and purified (FCC) to yield the title compound (66 mg, 72%).

후처리

  1. customTo a stirred rt
  2. temperatureAfter cooling to rt
  3. customthe catalyst was removed by filtration through a pad of celite
  4. washthe celite pad washed with MeOH
  5. concentrationThe filtrate was concentrated
  6. custompurified (FCC)

출처 및 근거

ORD 기록
ord-163a3eecfe3a49e2af091b8bf9e71ece
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08598202B2

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