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O-Methylhydroxylamine hydrochloride → HCID 178448679, 화합물

HRID 2235434
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HRID 2235434 반응식
[CH3:1][C:2]1([CH3:29])[C:10]2[CH:9]=[C:8]3[N:11]=[C:12]([NH:14][C:15](=[O:22])[C:16]4[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=4)[NH:13][C:7]3=[CH:6][C:5]=2[N:4]([CH2:23][C:24](=O)[CH2:25][CH3:26])[C:3]1=[O:28].Cl.[CH3:31][O:32][NH2:33]>CO>[CH3:31][O:32]/[N:33]=[C:24](/[CH2:25][CH3:26])\[CH2:23][N:4]1[C:5]2[CH:6]=[C:7]3[NH:13][C:12]([NH:14][C:15](=[O:22])[C:16]4[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=4)=[N:11][C:8]3=[CH:9][C:10]=2[C:2]([CH3:1])([CH3:29])[C:3]1=[O:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 178459291HCID 178459291, 화합물

생성물 1

HCID 178448679HCID 178448679, 화합물수율 66.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of N-[7,7-dimethyl-6-oxo-5-(2-oxo-butyl)-3,5,6,7-tetrahydro-imidazo[4,5-f]indol-2-yl]-benzamide (80 mg) in MeOH (20 ml) is added O-methyl-hydroxylamine hydrochloride (20.5 mg; 0.25 mmol) and the mixture is stirred at RT for 18 h. After evaporation EtOAc is added and the organic phase is washed three times with saturated K2CO3 solution, dried over MgSO4 and evaporated again. The residue is purified by RP-MPLC eluted with MeCN/water to yield the desired compound (57 mg).

후처리

  1. customAfter evaporation EtOAc
  2. additionis added
  3. washthe organic phase is washed three times with saturated K2CO3 solution
  4. dry with materialdried over MgSO4
  5. customevaporated again
  6. customThe residue is purified by RP-MPLC
  7. washeluted with MeCN/water

출처 및 근거

ORD 기록
ord-16df45b721f14ec59aa7b35a0c23afba
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07714010B2

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