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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acetic Acid → 1,1-Dimethylethyl 4-[5-[(1-methylethyl)amino]-4-pyrimidinyl]-1-piperazinecarboxylate

HRID 1449712
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HRID 1449712 반응식
C([BH3-])#N.[Na+].[CH3:5][C:6]([CH3:24])([O:8][C:9]([N:11]1[CH2:16][CH2:15][N:14]([C:17]2[N:22]=[CH:21][N:20]=[CH:19][C:18]=2[NH2:23])[CH2:13][CH2:12]1)=[O:10])[CH3:7].[CH3:25][C:26]([CH3:28])=O.C(O)(=O)C>CO.[OH-].[Na+].ClCCl>[CH3:7][C:6]([CH3:24])([O:8][C:9]([N:11]1[CH2:12][CH2:13][N:14]([C:17]2[N:22]=[CH:21][N:20]=[CH:19][C:18]=2[NH:23][CH:26]([CH3:28])[CH3:25])[CH2:15][CH2:16]1)=[O:10])[CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 176Acetic AcidHCID 180AcetoneHCID 5003444Sodium cyanoborohydrideHCID 21477601HCID 21477601, 화합물

생성물 1

HCID 214776211,1-Dimethylethyl 4-[5-[(1-methylethyl)amino]-4-pyrimidinyl]-1-piperazinecarboxylate

시약·촉매·용매 3

HCID 887Methanol용매2회
HCID 6344Dichloromethane용매
HCID 14798Sodium Hydroxide용매

실험 절차

A solution of sodium cyanoborohydride (0.13 g) in methanol (4 ml) is added to a mixture of 1-[1,1-dimethylethoxycarbonyl]-4-[5-amino-6-pyrimidinyl]piperazine (PREPARATION 10, 0.44 g), acetone (3 ml), and glacial acetic acid (0.4 ml) in methanol (7 ml) at 0°. The mixture is stirred at 20°-25° for 72h. The reaction is diluted with an aqueous sodium hydroxide solution (10%) and dichloromethane. The phases are separated and the organic phase is washed with water and the concentrated to a colorless liquid which is flash chromatographed on silica gel eluting with methanol/chloroform (1/99). The appropriate fractions are pooled and concentrated to give the title compound, NMR (CDCl3) 1.26, 1.49, 3.2, 3.44, 3.5-3.62, 7.89 and 8.33 δ.

후처리

  1. customThe phases are separated
  2. washthe organic phase is washed with water
  3. concentrationthe concentrated to a colorless liquid which
  4. customchromatographed on silica gel eluting with methanol/chloroform (1/99)
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e1fb7d40851e476280f139ac49c932c9
출처 데이터셋
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05599930

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