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Methyl iodide → HCID 87687587, 화합물

HRID 1396267
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HRID 1396267 반응식
[CH2:1]([O:8][C@@H:9]1[C@@H:17]([C@@H:18]([O:25][CH2:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH:19]2SCCCS2)[O:16][C@H:15]2[C@H:11]([N:12]=[C:13]([N:33]([CH3:35])[CH3:34])[S:14]2)[C@H:10]1[O:36][CH2:37][C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O-])([O-])=[O:45].[Ca+2].CI>CC(C)=O.O.ClCCl>[CH2:26]([O:25][C@H:18]([C@H:17]1[O:16][C@H:15]2[C@H:11]([N:12]=[C:13]([N:33]([CH3:35])[CH3:34])[S:14]2)[C@@H:10]([O:36][CH2:37][C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[C@@H:9]1[O:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[CH:19]=[O:45])[C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 6328Methyl iodideHCID 10112Calcium CarbonateHCID 86701113HCID 86701113, 화합물

생성물 1

HCID 87687587HCID 87687587, 화합물

시약·촉매·용매 3

HCID 180Acetone용매HCID 962Water용매
HCID 6344
Dichloromethane
용매

실험 절차

To a solution of 97 (3 g, 4.7 mmol) in acetone (16 mL) and water (4 mL) was added CaCO3 (4.7 g, 47 mmol) and CH3I (13.2 g, 94 mmol). After kept 20 hours at 50° C., the resulting solution was diluted with dichloromethane (30 mL), filtered and extracted with dichloromethane (2×30 mL). The combined organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to afford crude 98, which was used in next step directly; (ES, m/z) [M+H]+ 547.0.

후처리

  1. filtrationfiltered
  2. extractionextracted with dichloromethane (2×30 mL)
  3. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto afford crude 98, which

출처 및 근거

ORD 기록
ord-b187874fde164f169813de93bff8e180
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08901087B2

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