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Water → HCID 18548815, 화합물

HRID 1266894
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HRID 1266894 반응식
Cl[CH2:2][C:3]1[N:4]=[C:5]([C:8]2[CH:9]=[C:10]([C:14]3[CH2:20][C:19](=[O:21])[NH:18][C:17]4[CH:22]=[C:23]([N:26]5[CH:30]=[CH:29][CH:28]=[CH:27]5)[CH:24]=[CH:25][C:16]=4[N:15]=3)[CH:11]=[CH:12][CH:13]=2)[O:6][CH:7]=1.[I-].[K+].[CH3:33][NH2:34].O>C(O)C>[CH3:33][NH:34][CH2:2][C:3]1[N:4]=[C:5]([C:8]2[CH:9]=[C:10]([C:14]3[CH2:20][C:19](=[O:21])[NH:18][C:17]4[CH:22]=[C:23]([N:26]5[CH:30]=[CH:29][CH:28]=[CH:27]5)[CH:24]=[CH:25][C:16]=4[N:15]=3)[CH:11]=[CH:12][CH:13]=2)[O:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 4875Potassium IodideHCID 6329MethylamineHCID 18548707HCID 18548707, 화합물

생성물 1

HCID 18548815HCID 18548815, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
20 °C

실험 절차

A mixture of 4-[3-(4-chloromethyl-oxazol-2-yl)-phenyl]-8-pyrrol-1-yl-1,3-dihydro-benzo[b][1,4]diazepin-2-one (Example 78a) (125 mg) and potassium iodide (5 mg) in a 8M solution of methylamine in ethanol (1.5 mL) was stirred at 20° C. for 16 h. H2O (20 mL) was added and the precipitated collected by filtration and purified by chromatography on silica gel using MeOH as eluent. The product was stirred with 20% aqueous MeOH (10 mL) the pH of the mixture being set to 11 by addition of 1N NaOH solution, and the solid was isolated by filtration to give the title compound (54 mg) as yellow solid.

후처리

  1. filtrationthe precipitated collected by filtration
  2. custompurified by chromatography on silica gel
  3. stirringThe product was stirred with 20% aqueous MeOH (10 mL) the pH of the mixture
  4. additionbeing set to 11 by addition of 1N NaOH solution
  5. customthe solid was isolated by filtration

출처 및 근거

ORD 기록
ord-97834fb7a1dc4366b45c7c102231005d
출처 데이터셋
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06548495B2

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