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Hydrochloric Acid → HCID 178427600、化合物

HRID 367043
ノート
印刷プレビュー

反応式

HRID 367043 の反応式
[S:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.[Li]CCCC.[NH:11]([C:36]([O:38][C:39]([CH3:42])([CH3:41])[CH3:40])=[O:37])[C@H:12]([C:30](N(OC)C)=[O:31])[CH2:13][CH2:14][CH2:15][NH:16][C:17](=[NH:29])[NH:18][S:19]([C:22]1[CH:28]=[CH:27][C:25]([CH3:26])=[CH:24][CH:23]=1)(=[O:21])=[O:20].[Li]C1SC=CN=1.Cl.C1C[O:53]CC1>>[NH:11]([C:36]([O:38][C:39]([CH3:42])([CH3:40])[CH3:41])=[O:37])[C@H:12]([C:30]([OH:53])=[O:31])[CH2:13][CH2:14][CH2:15][NH:16][C:17](=[NH:29])[NH:18][S:19]([C:22]1[CH:28]=[CH:27][C:25]([CH3:26])=[CH:24][CH:23]=1)(=[O:20])=[O:21].[S:1]1[CH:5]=[CH:4][N:3]=[CH:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 6

HCID 313Hydrochloric AcidHCID 8028Tetrahydrofuran2 回HCID 9256ThiazoleHCID 178418339ButyllithiumHCID 178502742HCID 178502742、化合物HCID 178506781HCID 178506781、化合物

生成物 1

HCID 178427600
HCID 178427600、化合物
収率 84%

実験手順

To a solution of thiazole (2.5 g, 29 mmol) in THF (25 mL) at -78° C. was added n-BuLi (1.6 M in hexane, 19 mL) dropwise. The mixture was stirred for 30 minutes. Then a solution of Boc-Arg(Tos)-N(Me)OMe, from Example 1, (1.7 g, 3.6 mmol) in THF (50 mL) was added to the lithiothiazole mixture at -78° C. The solution was stirred for 2 hours. 1M HCl (30 mL) was added to the reaction mixture and warmed to room temperature. The mixture was extracted with EtOAc (100 mL). The organic layer was washed with sat. NaCl (30 mL), dried over MgSO4, filtered and evaporated. The crude oily residue was purified by flash column chromatography over SiO2 (50% EtOAc in CH2Cl2) to give Boc-Arg(Tos)-thiazole, shown above, (1.5 g, 84% yield) as a powder.

後処理

  1. stirringThe solution was stirred for 2 hours
  2. extractionThe mixture was extracted with EtOAc (100 mL)
  3. washThe organic layer was washed with sat. NaCl (30 mL)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated
  7. customThe crude oily residue was purified by flash column chromatography over SiO2 (50% EtOAc in CH2Cl2)

出典と根拠

ORDレコード
ord-92286d98c97f4cf6910b7c3ed6580957
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06133256

反応ノート

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