Tributyltin Chloride → HCID 22631454, 화합물

HRID 1840429노트

반응식

HRID 1840429 반응식
[CH2:1]([Sn:5](Cl)([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].C[Si]([N-][Si](C)(C)C)(C)C.[Li+].C1COCC1.[N+:30]([C:33]1[CH:55]=[CH:54][C:36]([CH2:37][O:38][C:39]([NH:41][CH2:42][CH2:43][CH2:44][S:45][C:46]2[N:47]=[CH:48][N:49]3[CH:53]=[CH:52][S:51][C:50]=23)=[O:40])=[CH:35][CH:34]=1)([O-:32])=[O:31].[Cl-].[NH4+]>C1COCC1>[N+:30]([C:33]1[CH:34]=[CH:35][C:36]([CH2:37][O:38][C:39]([NH:41][CH2:42][CH2:43][CH2:44][S:45][C:46]2[N:47]=[CH:48][N:49]3[CH:53]=[C:52]([Sn:5]([CH2:10][CH2:11][CH2:12][CH3:13])([CH2:6][CH2:7][CH2:8][CH3:9])[CH2:1][CH2:2][CH2:3][CH3:4])[S:51][C:50]=23)=[O:40])=[CH:54][CH:55]=1)([O-:32])=[O:31]

참가 물질

6

반응물 4

HCID 15096Tributyltin ChlorideHCID 25517Ammonium ChlorideHCID 22631774HCID 22631774, 화합물HCID 23714775LiHMDS tetrahydrofuran

생성물 1

HCID 22631454HCID 22631454, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Tri-n-butylstannyl chloride (1.21 ml) and 9.47 ml of a 1.0 N lithiumbis(trimethylsilyl)amide/THF solution were added to a solution of 1.11 g of 7-[3-(4-nitrobenzyloxycarbonyl)aminopropyl]thioimidazo[5,1-b]thiazole in 28 ml of THF at −45° C. under an argon atmosphere, and the mixture was stirred for one hr. An aqueous ammonium chloride solution was added to the reaction solution, and the mixture was extracted with ethyl acetate, followed by washing with brine. The organic layer was dried over anhydrous magnesium sulfate. The solvent was then removed by distillation, and the residue was purified by column chromatography on silica gel (hexane:ethyl acetate=1:1) to prepare 1.24 g of the title compound.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washby washing with brine
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. customThe solvent was then removed by distillation
  5. customthe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=1:1)
  6. customto prepare 1.24 g of the title compound

출처 및 근거

ORD 기록
ord-f2185ee6752942a8acf3812262fddafc
출처 데이터셋
uspto-grants-2004_01
특허 번호
US06680313B2

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