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Hydroxyamine hydrochloride → HCID 136335752, 화합물

HRID 2233941
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HRID 2233941 반응식
[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([CH3:8])[NH:4][C:3]=1[C:9]([NH:11][CH:12]1[CH2:17][CH2:16][N:15]([C:18]2[CH:23]=[C:22]([C:24]#[N:25])[CH:21]=[C:20]([Cl:26])[N:19]=2)[CH2:14][CH2:13]1)=[O:10].Cl.[NH2:28][OH:29]>CO>[NH2:25][C:24](=[N:28][OH:29])[C:22]1[CH:21]=[C:20]([Cl:26])[N:19]=[C:18]([N:15]2[CH2:14][CH2:13][CH:12]([NH:11][C:9]([C:3]3[NH:4][C:5]([CH3:8])=[C:6]([Cl:7])[C:2]=3[Cl:1])=[O:10])[CH2:17][CH2:16]2)[CH:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 86608292HCID 86608292, 화합물

생성물 1

HCID 136335752HCID 136335752, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

3,4-Dichloro-N-[1-(6-chloro-4-cyanopyridin-2-yl)piperidin-4-yl]-5-methyl-1H-pyrrole-2-carboxamide (Example 95; 150 mg, 0.362 mmol) was dissolved in MeOH (5 ml) and TEA (100 μl, 0.724 mmol) was added. Hydroxylamine hydrochloride (25.2 mg, 0.362 mmol) was added and the mixture was refluxed for 1 h. The solvent was removed in vacuo and the resulting precipitate was dissolved in DMSO and purified by semi preparative reverse phase HPLC eluting with CH3CN/H2O (0.1% TFA). (80 mg).

후처리

  1. temperaturethe mixture was refluxed for 1 h
  2. customThe solvent was removed in vacuo
  3. dissolutionthe resulting precipitate was dissolved in DMSO
  4. custompurified by semi preparative reverse phase HPLC
  5. washeluting with CH3CN/H2O (0.1% TFA)

출처 및 근거

ORD 기록
ord-a79ed01317ba41c1a208e02bc1062618
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07709503B2

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