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Chlorosuccinimide → 1-[2-chloro-3-(2,4-dichlorophenyl)-3-oxo-2-phenylpropyl]-N-[(1,1-dimethylethoxy)carbonyl]-L-histidine

HRID 34490
ノート
印刷プレビュー

反応式

HRID 34490 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9](=[O:36])[CH:10]([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[CH2:11][N:12]1[CH:29]=[N:28][C:14]([CH2:15][C@@H:16]([C:25]([OH:27])=[O:26])[NH:17][C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])=[CH:13]1.C[Si](C)(C)[N-][Si](C)(C)C.[Li+].[Cl:47]N1C(=O)CCC1=O>O1CCCC1.C(OCC)(=O)C>[Cl:47][C:10]([C:30]1[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1)([C:9]([C:3]1[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=1[Cl:1])=[O:36])[CH2:11][N:12]1[CH:29]=[N:28][C:14]([CH2:15][C@@H:16]([C:25]([OH:27])=[O:26])[NH:17][C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])=[CH:13]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 31398ChlorosuccinimideHCID 2733832Lithium hexamethyldisilazaneHCID 541777141-[3-(2,4-dichlorophenyl)-3-oxo-2-phenylpropyl]-N-[(1,1-dimethylethoxy)carbonyl]-L-histidine

生成物 1

HCID 228392281-[2-chloro-3-(2,4-dichlorophenyl)-3-oxo-2-phenylpropyl]-N-[(1,1-dimethylethoxy)carbonyl]-L-histidine収率 48.7%

試薬・触媒・溶媒 2

HCID 8028
Tetrahydrofuran
溶媒
3 回
HCID 8857Ethyl Acetate溶媒

実験手順

A portion of the 1-[3-(2,4-dichlorophenyl)-3-oxo-2-phenylpropyl]-N-[(1,1-dimethylethoxy)carbonyl]-L-histidine (5.5 g) in dry tetrahydrofuran (50 ml) was added dropwise to a stirred solution of lithium hexamethyldisilazide in tetrahydrofuran (33 ml, 1M solution in tetrahydrofuran) at -78° C. under an atmosphere of nitrogen. After 30 minutes the resulting solution was rapidly transferred, under an atmosphere of nitrogen, into a stirred solution of N-chlorosuccinimide (1.6 g) in dry tetrahydrofuran (50 ml). The resulting mixture was cooled in an ice bath under an atmosphere of nitrogen. The mixture was allowed to warm to room temperature over a period of 20 minutes and was quenched upon an addition of an excess of saturated aqueous potassium dihydrogen orthophosphate. The organic phase was separated and the aqueous phase was extracted twice with ethyl acetate. The organic phases were combined, dried over anhydrous magnesium sulphate and concentrated under reduced pressure to yield a residue. The residue was dissolved in ethyl acetate, washed with water and then brine, dried over anhydrous magnesium sulphate and concentrated under reduced pressure to yield a foam which was chromatographed on silica gel using a mixture of methanol:dichloromethane (2:23) as an eluent to yield 1-[2-chloro-3-(2,4-dichlorophenyl)-3-oxo-2-phenylpropyl]-N-[ (1,1-dimethylethoxy)carbonyl]-L-histidine (2.85 g) as a mixture of diastereoisomers, (δ (CDCl3) 1.45 (9H, s), 1.48 (9H, s), 3.01 (2H, bd, J=15Hz), 3.23 (2H, bd, J=15Hz), 4.35 (2H, bs), 4.62 (2H, bt, J=17Hz), 4.86 (2H, bt, J=17Hz), 5.48 (2H, m, 4 lines), 6.38 (1H, bs), 6.57 (3H, m), 6.98 (2H, dd, J=9Hz and 2Hz), 7.42 (2H, m), 7.46 (5H, s), 7.49 (5H, s), 7.56 (1H, bs) and 7.60 (1H, bs)), having the formula: ##STR33##

後処理

  1. temperatureThe resulting mixture was cooled in an ice bath under an atmosphere of nitrogen
  2. customwas quenched upon an addition of an excess of saturated aqueous potassium dihydrogen orthophosphate
  3. customThe organic phase was separated
  4. extractionthe aqueous phase was extracted twice with ethyl acetate
  5. dry with materialdried over anhydrous magnesium sulphate
  6. concentrationconcentrated under reduced pressure
  7. customto yield a residue
  8. washwashed with water
  9. dry with materialbrine, dried over anhydrous magnesium sulphate
  10. concentrationconcentrated under reduced pressure
  11. customto yield a foam which
  12. customwas chromatographed on silica gel using
  13. additiona mixture of methanol:dichloromethane (2:23) as an eluent

出典と根拠

ORDレコード
ord-58aee43308b54c6ba6cf6bfb4af7ac04
出典データセット
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04761483

反応ノート

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