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Tri(butyl)vinyltin → HCID 68456961, 화합물

HRID 2358416
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HRID 2358416 반응식
[C:1]([O:5][C:6](=[O:19])[NH:7][CH2:8][C:9]1[CH:14]=[C:13](I)[C:12]([NH2:16])=[CH:11][C:10]=1[O:17][CH3:18])([CH3:4])([CH3:3])[CH3:2].[CH2:20](C([Sn])=C(CCCC)CCCC)[CH2:21]CC>C1(C)C=CC=CC=1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:1]([O:5][C:6](=[O:19])[NH:7][CH2:8][C:9]1[CH:14]=[C:13]([CH:20]=[CH2:21])[C:12]([NH2:16])=[CH:11][C:10]=1[O:17][CH3:18])([CH3:4])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 53438229Tri(butyl)vinyltinHCID 68454768HCID 68454768, 화합물

생성물 1

HCID 68456961HCID 68456961, 화합물수율 43%

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매HCID 1140Toluene용매

실험 절차

To a solution of (4-amino-5-iodo-2-methoxy-benzyl)-carbamic acid tert-butyl ester (700 mg, 1.85 mmol) and tributylvinyltin (783 mg, 2.68 mmol) in toluene was added Pd(PPh3)4 (214 mg, 0.19 mmol) under argon. The resulting mixture was heated with reflux for 8 hrs, filtered through celite, and then concentrated under reduced pressure. The crude residue was column-chromatographed (hexane/ethylacetate=2/1 to 1/1) to yield (4-amino-2-methoxy-5-vinyl-benzyl)-carbamic acid tert-butyl ester (220 mg, 43%).

후처리

  1. temperatureThe resulting mixture was heated
  2. temperaturewith reflux for 8 hrs
  3. filtrationfiltered through celite
  4. concentrationconcentrated under reduced pressure
  5. customThe crude residue was column-chromatographed (hexane/ethylacetate=2/1 to 1/1)

출처 및 근거

ORD 기록
ord-61f3831ae69d49e1a711d09daa74c42f
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07763657B2

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