Triethylamine → ((E)-3-{3-Benzyloxy-4-[1,1,4-trioxo-5-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-2-yl]-phenyl}-1,1-dimethylallyl)-carbamic Acid Tert-butyl Ester

HRID 660524노트

반응식

HRID 660524 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[C:13](I)[CH:12]=[CH:11][C:10]=1[N:16]1[S:20](=[O:22])(=[O:21])[N:19]([CH2:23][CH2:24][Si:25]([CH3:28])([CH3:27])[CH3:26])[C:18](=[O:29])[CH2:17]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:30]([O:34][C:35](=[O:42])[NH:36][C:37]([CH3:41])([CH3:40])[CH:38]=[CH2:39])([CH3:33])([CH3:32])[CH3:31].C(N(CC)CC)C>CN(C=O)C>[C:30]([O:34][C:35](=[O:42])[NH:36][C:37]([CH3:41])([CH3:40])/[CH:38]=[CH:39]/[C:13]1[CH:12]=[CH:11][C:10]([N:16]2[CH2:17][C:18](=[O:29])[N:19]([CH2:23][CH2:24][Si:25]([CH3:28])([CH3:27])[CH3:26])[S:20]2(=[O:22])=[O:21])=[C:9]([O:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH:14]=1)([CH3:33])([CH3:32])[CH3:31]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 13294366(1,1-Dimethylallyl)carbamic acid tert-butyl esterHCID 667569375-(2-Benzyloxy-4-iodophenyl)-1,1-dioxo-2-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-3-one

생성물 1

HCID 68839103((E)-3-{3-Benzyloxy-4-[1,1,4-trioxo-5-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-2-yl]-phenyl}-1,1-dimethylallyl)-carbamic Acid Tert-butyl Ester

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

To a solution of 5-(2-benzyloxy-4-iodophenyl)-1,1-dioxo-2-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-3-one (1.4 g, 3 mmol) in DMF (20 mL) is added (1,1-dimethylallyl)-carbamic acid tert-butyl ester (560 mg, 3 mmol), triethylamine (0.7 mL, 5 mmol) and tert-di(mu-acetato) bis[o-(di-o-tolylphosphino)benzyl]dipalladium (II) (25 mg). The mixture is stirred at 80° C. for 18 h. The solvent is removed under reduced pressure and the residue is purified by flash chromatography to give the title compound

후처리

  1. customThe solvent is removed under reduced pressure
  2. customthe residue is purified by flash chromatography

출처 및 근거

ORD 기록
ord-a722fbd296ba4a7f9de580978838d3de
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084448B2

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