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Acetic Acid → HCID 68762386, 화합물

HRID 1398818
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HRID 1398818 반응식
[NH2:1][C:2]1[C:7]2[N:8]([CH2:22][CH2:23][CH2:24][OH:25])[C:9]([NH:11][C:12]3[C:13]([O:20][CH3:21])=[N:14][C:15]([O:18][CH3:19])=[N:16][CH:17]=3)=[N:10][C:6]=2[CH:5]=[CH:4][CH:3]=1.[CH:26](=O)[CH3:27].[C:29](O)(=O)[CH3:30].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)(O)[O-].[Na+]>O1CCCC1>[CH2:29]([N:1]([CH2:26][CH3:27])[C:2]1[C:7]2[N:8]([CH2:22][CH2:23][CH2:24][OH:25])[C:9]([NH:11][C:12]3[C:13]([O:20][CH3:21])=[N:14][C:15]([O:18][CH3:19])=[N:16][CH:17]=3)=[N:10][C:6]=2[CH:5]=[CH:4][CH:3]=1)[CH3:30]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 176Acetic AcidHCID 177AcetaldehydeHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 68766787HCID 68766787, 화합물

생성물 1

HCID 68762386HCID 68762386, 화합물수율 78%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

실험 절차

To a mixture of 3-{7-amino-2-[(2,4-dimethoxypyrimidin-5-yl)amino]-1H-benzimidazol-1-yl}propan-1-ol (99 mg, 0.287 mmol), acetaldehyde (90%, 0.178 mL, 2.87 mmol) and acetic acid (0.066 mL, 1.15 mmol) in tetrahydrofuran (2.0 mL) was added sodium triacetoxyborohydride (384 mg, 1.72 mmol) portionwise at 0° C. The mixture was warmed to room temperature and stirred for 14 hr. Aqueous sodium bicarbonate was added and the mixture was extracted with ethyl acetate. Organic layer was washed with brine, dried over sodium sulfate and concentrated in vacuo. The residue was purified by flash chromatography on silica gel eluting with a 50-100% ethyl acetate/n-hexane gradient mixture. The filtrate was concentrated in vacuo to give the title compound (90 mg, 0.224 mmol, 78%) as a colorless amorphous.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washOrganic layer was washed with brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by flash chromatography on silica gel eluting with a 50-100% ethyl acetate/n-hexane gradient mixture
  6. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-e709efd4a95640d8a68b86ec6fc16d93
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08901141B2

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