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Cyanogen Bromide → HCID 11248809, 화합물

HRID 1866861
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HRID 1866861 반응식
C(=O)(O)[O-].[Na+].[C:6]1([C:12]2([C:19]3[CH:28]=[C:27]([O:29][CH2:30][C:31]4[CH:40]=[CH:39][C:38]5[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=5)[N:32]=4)[CH:26]=[CH:25][C:20]=3[C:21]([NH:23][NH2:24])=[O:22])[CH2:17][CH:16]3[CH2:18][CH:13]2[CH2:14][CH2:15]3)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[N:41]#[C:42]Br>O.O1CCOCC1>[C:6]1([C:12]2([C:19]3[CH:28]=[C:27]([O:29][CH2:30][C:31]4[CH:40]=[CH:39][C:38]5[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=5)[N:32]=4)[CH:26]=[CH:25][C:20]=3[C:21]3[O:22][C:42]([NH2:41])=[N:24][N:23]=3)[CH2:17][CH:16]3[CH2:18][CH:13]2[CH2:14][CH2:15]3)[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 10476Cyanogen BromideHCID 516892Sodium Bicarbonate2회HCID 57978651HCID 57978651, 화합물

생성물 1

HCID 11248809HCID 11248809, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매2회

실험 절차

A solution of sodium bicarbonate (10.0 mg, 0.12 mmol) in water (267 μL) was added dropwise via syringe to a stirred solution of 4d (0.108 mmol) in dioxane (1.0 mL) at room temperature. A suspension of cyanogen bromide (13.0 mg, 0.12 mmol) in dioxane (120 μL) was added in 4 equal portions at 1 minute intervals. After approximately 45 min, the reaction mixture was poured into saturated aqueous sodium bicarbonate and extracted three times with methylene chloride. The combined organic extracts were washed with brine, dried (Na2SO4) and concentrated in vacuo. The crude residue was purified by preparative reversed phase HPLC on YMC Pack Pro C18 stationary phase (gradient elution; 0-75% acetonitrile/water as eluent, 0.1% TiFA as modifier). Lyophilization of the purified fractions afforded the title compound 5b, m/z (ES) 489 (MH)+.

후처리

  1. additionwas added in 4 equal portions at 1 minute intervals
  2. extractionextracted three times with methylene chloride
  3. washThe combined organic extracts were washed with brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated in vacuo
  6. customThe crude residue was purified by preparative reversed phase HPLC on YMC Pack Pro C18 stationary phase (gradient elution; 0-75% acetonitrile/water as eluent, 0.1% TiFA as modifier)

출처 및 근거

ORD 기록
ord-fc8d250865794ca79ddc3586c1eafbec
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07629467B2

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