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Phthalimide → HCID 66975369、化合物

HRID 1022591
ノート
印刷プレビュー

反応式

HRID 1022591 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([CH2:23]O)[O:15][CH2:14][CH2:13][N:12]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].[C:25]1(=[O:35])[NH:29][C:28](=[O:30])[C:27]2=[CH:31][CH:32]=[CH:33][CH:34]=[C:26]12.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>C1COCC1.C1(C)C=CC=CC=1.O>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([CH2:23][N:29]3[C:25](=[O:35])[C:26]4[C:27](=[CH:31][CH:32]=[CH:33][CH:34]=4)[C:28]3=[O:30])[O:15][CH2:14][CH2:13][N:12]([C:16]([O:18][C:19]([CH3:20])([CH3:21])[CH3:22])=[O:17])[CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]
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 6809Phthalimide2 回HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamate2 回HCID 66975608HCID 66975608、化合物

生成物 1

HCID 66975369HCID 66975369、化合物収率 55.5%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 1140Toluene溶媒2 回
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

To a solution of tert-butyl (7RS)-7-(3,4-dichlorophenyl)-7-(hydroxymethyl)-1,4-oxazepane-4-carboxylate (2 g), phthalimide (0.86 g) and triphenylphosphine (4.17 g) in THF (40 ml) was added dropwise a solution (2.2 M, 7.2 ml) of diethyl azodicarboxylate in toluene at 0° C., and the mixture was stirred at 0° C. for 30 min, and then for 6 hr while warming to room temperature. To the reaction mixture were added phthalimide (0.43 g) and a solution (2.2 M, 3.6 mL) of diethyl azodicarboxylate in toluene, and the mixture was stirred at room temperature for 14 hr. The reaction mixture was diluted with water, and the mixture was extracted with ethyl acetate. The obtained extract was washed with brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (ethyl acetate/hexane) and silica gel column chromatography (NH, ethyl acetate/hexane) to give the title compound (1.49 g).

後処理

  1. temperaturefor 6 hr while warming to room temperature
  2. extractionthe mixture was extracted with ethyl acetate
  3. extractionThe obtained extract
  4. washwas washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customThe obtained residue was purified by silica gel column chromatography (ethyl acetate/hexane) and silica gel column chromatography (NH, ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-fba7353ec01b49359ab60ce6596c83a4
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08722662B2

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