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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ammonium Acetate → HCID 22458318, 화합물

HRID 2184925
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HRID 2184925 반응식
C([NH:5][S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:15]1[CH:20]=[CH:19][C:18]([NH:21][C:22]([C:24]2[CH2:28][CH2:27][CH2:26][C:25]=2[C:29]2[CH:34]=[CH:33][CH:32]=[C:31]([C:35]#[N:36])[CH:30]=2)=[O:23])=[CH:17][CH:16]=1)(=[O:8])=[O:7])(C)(C)C.C([O-])(=O)C.[NH4+:41]>CO>[S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:15]1[CH:16]=[CH:17][C:18]([NH:21][C:22]([C:24]2[CH2:28][CH2:27][CH2:26][C:25]=2[C:29]2[CH:30]=[C:31]([C:35]([NH2:41])=[NH:36])[CH:32]=[CH:33][CH:34]=2)=[O:23])=[CH:19][CH:20]=1)(=[O:8])(=[O:7])[NH2:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 22458356HCID 22458356, 화합물

생성물 1

HCID 22458318HCID 22458318, 화합물수율 63.4%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To a solution of N-[4-(2-{[(tert-butyl)amino]sulfonyl}phenyl)phenyl][2-(3-cyanophenyl)cyclopent-1-enyl]carboxamide (70 mg, 0.137 mmol) in 5 ml anhydrous methanol cooled in an ice bath was bubbled HCl gas until saturation was achieved. Reaction was allowed to warm to room temperature and stirred overnight. The reaction was then concentrated in vacuo and dried under hi vacuum. The dried residue was dissolved in 5 ml anhydrous methanol to which ammonium acetate (77 mg, 1 mmol) was added and the reaction heated to reflux for 2 hours. The reaction was concentrated and purified on a 2×25 cm Vydac C18 HPLC column to give 3-(2-{N-[4-(2-sulfamoylphenyl)phenyl]carbamoyl}cyclopent-1-enyl)benzenecarboxamidine (40 mg, 63%) as a fluffy white powder after lyophilization. ES-MS (M+H+): 461.15

후처리

  1. customwas bubbled HCl gas until saturation
  2. customReaction
  3. concentrationThe reaction was then concentrated in vacuo
  4. customdried under hi vacuum
  5. additionwas added
  6. temperaturethe reaction heated
  7. temperatureto reflux for 2 hours
  8. concentrationThe reaction was concentrated
  9. custompurified on a 2×25 cm Vydac C18 HPLC column

출처 및 근거

ORD 기록
ord-16402d90b48142478d7c2d672e41f70e
출처 데이터셋
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06399627B1

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