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Chlorotrimethylsilane → HCID 22870460, 화합물

HRID 976021
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HRID 976021 반응식
Cl.Cl.[NH2:3][C@@H:4]([CH2:8]/[CH:9]=[CH:10]/[CH2:11][C@H:12]([NH2:16])[C:13]([OH:15])=[O:14])[C:5]([OH:7])=[O:6].C[Si](Cl)(C)C.[C:22](Cl)([O:24][CH2:25][CH:26]1[C:38]2[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=2)[C:32]2[C:27]1=[CH:28][CH:29]=[CH:30][CH:31]=2)=[O:23]>C[Si](N[Si](C)(C)C)(C)C.ClCCl>[CH:37]1[C:38]2[CH:26]([CH2:25][O:24][C:22]([NH:3][C@@H:4]([CH2:8]/[CH:9]=[CH:10]/[CH2:11][C@H:12]([NH:16][C:22]([O:24][CH2:25][CH:26]3[C:27]4[CH:28]=[CH:29][CH:30]=[CH:31][C:32]=4[C:33]4[C:38]3=[CH:37][CH:36]=[CH:35][CH:34]=4)=[O:23])[C:13]([OH:15])=[O:14])[C:5]([OH:7])=[O:6])=[O:23])[C:27]3[C:32](=[CH:31][CH:30]=[CH:29][CH:28]=3)[C:33]=2[CH:34]=[CH:35][CH:36]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6397ChlorotrimethylsilaneHCID 343679-Fluorenylmethyl chloroformateHCID 86750549HCID 86750549, 화합물

생성물 1

HCID 22870460HCID 22870460, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 13838Hexamethyldisilazane용매

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온도
0 °C

실험 절차

(S,S)-2,7-Diamino-E-oct-4-enedioic acid dihydrochloride (1.59 g, 5.8 mmol) was suspended in HMDS (20 ml) and TMSCl and refluxed overnight. The solvents were removed, and the residue was dissolved in anhydrous dichloromethane. This solution was cooled to 0° C. and a solution of FmocCl (3.10 g, 12 mmol) in dichloromethane was added. The solution was stirred for 1 hour at this temperature and overnight at ambient temperature. The solvent was evaporated and the residue dissolved in THF. After addition of 1N aqueous HCl the solution was stirred for two hours, extracted with chloroform and dried (MgSO4). The residue was dissolved in dichloromethane and crystallized by the addition of diethylether.

후처리

  1. customThe solvents were removed
  2. dissolutionthe residue was dissolved in anhydrous dichloromethane
  3. customThe solvent was evaporated
  4. dissolutionthe residue dissolved in THF
  5. additionAfter addition of 1N aqueous HCl the solution
  6. stirringwas stirred for two hours
  7. extractionextracted with chloroform
  8. dry with materialdried (MgSO4)
  9. dissolutionThe residue was dissolved in dichloromethane
  10. customcrystallized by the addition of diethylether

출처 및 근거

ORD 기록
ord-feac30f1e166451c8b7e4bf428483f7b
출처 데이터셋
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05610141

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