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Triethylamine → (S)-3-((E)-2-{3-Benzyloxy-4-[1,1,4-trioxo-5-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-2-yl]-phenyl}-vinyl)-3,4-dihydro-1H-isoquinoline-2-carboxylic Acid Tert-butyl Ester

HRID 660662
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HRID 660662 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]([N:37]1[C@H:46]([CH:47]=[CH2:48])[CH2:45][C:44]2[C:39](=[CH:40][CH:41]=[CH:42][CH:43]=2)[CH2:38]1)=[O:36])([CH3:33])([CH3:32])[CH3:31].CCN(CC)CC.C(C1C=CC(C2C=CC=CC=2)=C(P)C=1C(C)(C)C)(C)(C)C>C(#N)C.Cl.CC([O-])=O.CC([O-])=O.[Pd+2]>[C:30]([O:34][C:35]([N:37]1[C@H:46](/[CH:47]=[CH:48]/[C:13]2[CH:12]=[CH:11][C:10]([N:16]3[CH2:17][C:18](=[O:29])[N:19]([CH2:23][CH2:24][Si:25]([CH3:28])([CH3:27])[CH3:26])[S:20]3(=[O:22])=[O:21])=[C:9]([O:8][CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[CH:14]=2)[CH2:45][C:44]2[C:39](=[CH:40][CH:41]=[CH:42][CH:43]=2)[CH2:38]1)=[O:36])([CH3:33])([CH3:32])[CH3:31]
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참가 물질

8

반응물 4

HCID 8471TriethylamineHCID 21864676Di-t-butyl-phosphinobiphenylHCID 667569375-(2-Benzyloxy-4-iodophenyl)-1,1-dioxo-2-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-3-oneHCID 68838676(S)-3-Vinyl-3,4-dihydro-1H-isoquinoline-2-carboxylic Acid Tert-butyl Ester

생성물 1

HCID 68996827
(S)-3-((E)-2-{3-Benzyloxy-4-[1,1,4-trioxo-5-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-2-yl]-phenyl}-vinyl)-3,4-dihydro-1H-isoquinoline-2-carboxylic Acid Tert-butyl Ester

시약·촉매·용매 3

HCID 167845palladium(II) acetate촉매HCID 313Hydrochloric Acid용매HCID 6342Acetonitrile용매

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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 (0.77 g, 1.4 mmol) and (S)-3-vinyl-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester (0.44 g, 1.7 mmol) in acetonitrile (5 mL) in a pressure vessel is added Et3N (0.32 mL, 2.3 mmol) followed by di-t-butyl-phosphinobiphenyl (0.017 g, 0.057 mmol). The solution is degassed by nitrogen sparging for 10 min, and then Pd(OAc)2 (0.006 g, 0.028 mmol) is added and the mixture is heated to 80° C. for 18 h. The mixture is cooled to RT and is diluted with 1N HCl and extracted with EtOAc (2×30 mL). The organic layer is washed with brine (3×30 mL) and dried over Na2SO4. The solvent is removed under reduced pressure and the residue purified by flash chromatography using a gradient of 5 to 30% EtOAc in hexanes to give the title compound.

후처리

  1. customThe solution is degassed by nitrogen sparging for 10 min
  2. temperatureThe mixture is cooled to RT
  3. extractionextracted with EtOAc (2×30 mL)
  4. washThe organic layer is washed with brine (3×30 mL)
  5. dry with materialdried over Na2SO4
  6. customThe solvent is removed under reduced pressure
  7. customthe residue purified by flash chromatography

출처 및 근거

ORD 기록
ord-f9bda00b05cc4bf7a7c90c1c267a46cf
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08084448B2

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