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Dibutyltin oxide → HCID 178460975, 화합물

HRID 1921897
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HRID 1921897 반응식
[C:1]([C:5]1[CH:51]=[CH:50][C:8]([CH2:9][O:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2/[CH:17]=[CH:18]/[CH:19]([CH2:30][C:31]2[CH:36]=[C:35]([F:37])[C:34]([O:38][Si:39]([CH:46]([CH3:48])[CH3:47])([CH:43]([CH3:45])[CH3:44])[CH:40]([CH3:42])[CH3:41])=[C:33]([F:49])[CH:32]=2)[CH2:20][CH2:21][C:22]2[CH:29]=[CH:28][C:25]([C:26]#[N:27])=[CH:24][CH:23]=2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].C[Si]([N:56]=[N+:57]=[N-:58])(C)C.C([Sn](=O)CCCC)CCC>C1(C)C=CC=CC=1>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([CH2:9][O:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2/[CH:17]=[CH:18]/[CH:19]([CH2:30][C:31]2[CH:32]=[C:33]([F:49])[C:34]([O:38][Si:39]([CH:40]([CH3:42])[CH3:41])([CH:43]([CH3:44])[CH3:45])[CH:46]([CH3:48])[CH3:47])=[C:35]([F:37])[CH:36]=2)[CH2:20][CH2:21][C:22]2[CH:29]=[CH:28][C:25]([C:26]3[NH:58][N:57]=[N:56][N:27]=3)=[CH:24][CH:23]=2)=[CH:50][CH:51]=1)([CH3:4])([CH3:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 61221Dibutyltin oxideHCID 78378AzidotrimethylsilaneHCID 57971908E-4-[5-[2-(4-tert-Butylbenzyloxy)phenyl]-3-(3,5-difluoro-4-triisopropylsilanyloxybenzyl)pent-4-enyl]benzonitrile

생성물 1

HCID 178460975HCID 178460975, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
80 °C

실험 절차

A solution of 625 mg (85% pure, 0.75 mmol) of E-4-[5-[2-(4-tert-butylbenzyloxy)phenyl]-3-(3,5-difluoro-4-triisopropylsilanyloxybenzyl)pent-4-enyl]benzonitrile in 12 ml of toluene is mixed with 1.76 ml (13.24 mmol) of trimethylsilyl azide and 329.6 mg (1.3 mmol) of di-n-butyltin oxide and stirred at 80° C. for 12 h. After conversion is complete, the mixture is extracted with sodium bicarbonate solution. The aqueous phase is back-extracted twice with ethyl acetate. The combined organic phases are washed with sodium chloride solution, dried over sodium sulfate and concentrated. The resulting residue is purified by flash chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 1:2→ethyl acetate). 447.3 mg (0.51 mmol, 86% purity, 58% of theory) of the title compound are obtained.

후처리

  1. extractionthe mixture is extracted with sodium bicarbonate solution
  2. extractionThe aqueous phase is back-extracted twice with ethyl acetate
  3. washThe combined organic phases are washed with sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customThe resulting residue is purified by flash chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 1:2→ethyl acetate)

출처 및 근거

ORD 기록
ord-8d834509c16e48ed954db95eca912a6b
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08173704B2

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