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Chlorotrimethylsilane → HCID 22870460、化合物

HRID 976021
ノート
印刷プレビュー

反応式

HRID 976021 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6397ChlorotrimethylsilaneHCID 343679-Fluorenylmethyl chloroformateHCID 86750549HCID 86750549、化合物

生成物 1

HCID 22870460HCID 22870460、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 13838Hexamethyldisilazane溶媒

反応条件

温度
0 °C

実験手順

(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.

後処理

  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

出典と根拠

ORDレコード
ord-feac30f1e166451c8b7e4bf428483f7b
出典データセット
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05610141

反応ノート

読み込み中…

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