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Methyl iodide → HCID 58484975, 화합물

HRID 1255440
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HRID 1255440 반응식
[H-].[Na+].[Cl:3][C:4]1[N:5]=[CH:6][C:7]2[NH:13][C:12](=[O:14])[C:11]3([CH2:16][CH2:15]3)[CH2:10][N:9]([C@@H:17]3[CH2:21][CH2:20][C:19]([F:23])([F:22])[CH2:18]3)[C:8]=2[N:24]=1.[CH3:25]I>>[Cl:3][C:4]1[N:5]=[CH:6][C:7]2[N:13]([CH3:25])[C:12](=[O:14])[C:11]3([CH2:16][CH2:15]3)[CH2:10][N:9]([C@@H:17]3[CH2:21][CH2:20][C:19]([F:23])([F:22])[CH2:18]3)[C:8]=2[N:24]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 86658721HCID 86658721, 화합물

생성물 1

HCID 58484975HCID 58484975, 화합물수율 92%

실험 절차

60% sodium hydride in mineral oil (0.25 g, 6.23 mmol) was added to a mixture of (R)-2′-chloro-9′-(3,3-difluorocyclopentyl)-8′,9′-dihydrospiro[cyclopropane-1,7′-pyrimido[4,5-b][1,4]diazepin]-6′(5′H)-one (1.95 g, 5.94 mmol) and methyl iodide (0.41 ml, 6.53 mmol) dimethylacetamide (20 mL). The reaction mixture was stirred at room temperature for 25 minutes. Ice was added to the reaction mixture. A solid crashed out and was filtered off, rinsing with water. The solid was dried in a pistol under vacuo for 3 hours. The compound was obtained as a light pink solid (1.863 g, 92% yield).

후처리

  1. additionIce was added to the reaction mixture
  2. filtrationwas filtered off
  3. washrinsing with water
  4. customThe solid was dried in a pistol under vacuo for 3 hours

출처 및 근거

ORD 기록
ord-fe85da98c9234e5e97fa3dcac2a94f51
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08461149B2

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