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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
ノート
印刷プレビュー

反応式

HRID 660662 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 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

生成物 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

試薬・触媒・溶媒 3

HCID 167845palladium(II) acetate触媒HCID 313Hydrochloric Acid溶媒HCID 6342Acetonitrile溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f9bda00b05cc4bf7a7c90c1c267a46cf
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08084448B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート