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Bromotrimethylsilane → HCID 70091067, 화합물

HRID 2395252
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HRID 2395252 반응식
C([O:3][P:4]([CH2:9][CH2:10][NH:11][S:12]([CH2:15][CH2:16][CH2:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[O:25][CH2:26][CH2:27][CH2:28][CH2:29][CH:30]1[CH2:35][CH2:34][N:33](C(OC(C)(C)C)=O)[CH2:32][CH2:31]1)(=[O:14])=[O:13])(=[O:8])[O:5]CC)C.C[Si](Br)(C)C.CCO.[NH4+].[OH-].O>C(Cl)(Cl)Cl>[NH:33]1[CH2:34][CH2:35][CH:30]([CH2:29][CH2:28][CH2:27][CH2:26][O:25][C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2[CH2:18][CH2:17][CH2:16][CH2:15][S:12]([NH:11][CH2:10][CH2:9][P:4]([OH:8])(=[O:3])[OH:5])(=[O:14])=[O:13])[CH2:31][CH2:32]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 76113BromotrimethylsilaneHCID 86596525Ethanol ammonium hydroxide waterHCID 86751156HCID 86751156, 화합물

생성물 1

HCID 70091067HCID 70091067, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A solution of 6-9 (0.63 g, 0.142 mmol) in CHCl3 (5 ml) at rt was treated with TMSBr (0.85 mmol) for 16 hrs. The solvent was removed and the residue was dissolved in 10% aqueous acetone and this stripped to dryness. The residue was mixed with toluene and the resulting gum was purified by flash chromatography on silica gel eluting with 4:1:1 EtOH/H2 O/NH4OH to provide pure 6-11. Rf 0.38 (silica gel, 4:1:1 EtOH/NH4OH/H2O. ##STR61##

후처리

  1. customThe solvent was removed
  2. dissolutionthe residue was dissolved in 10% aqueous acetone
  3. additionThe residue was mixed with toluene
  4. customthe resulting gum was purified by flash chromatography on silica gel eluting with 4:1:1 EtOH/H2 O/NH4OH
  5. customto provide pure 6-11

출처 및 근거

ORD 기록
ord-093f8ca82d1d4d6d97f70f51cfcc7cb6
출처 데이터셋
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05814643

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