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Tetrahydrofuran → HCID 68530764、化合物

HRID 1967421
ノート
印刷プレビュー

反応式

HRID 1967421 の反応式
[NH2:1][N:2]1[C:6](=[O:7])[C:5]2=[CH:8][CH:9]=[CH:10][CH:11]=[C:4]2[C:3]1=[O:12].O1CCCC1.[CH3:18][C:19]([CH3:29])([CH2:27][CH3:28])[CH:20]([CH2:23][C:24](=O)[CH3:25])[CH:21]=O>Cl.C(OCC)(=O)C>[CH3:18][C:19]([C:20]1[CH:23]=[C:24]([CH3:25])[N:1]([N:2]2[C:3](=[O:12])[C:4]3[C:5](=[CH:8][CH:9]=[CH:10][CH:11]=3)[C:6]2=[O:7])[CH:21]=1)([CH3:29])[CH2:27][CH3:28]
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 8028TetrahydrofuranHCID 74645N-AminophthalimideHCID 86642084HCID 86642084、化合物

生成物 1

HCID 68530764HCID 68530764、化合物収率 77.6%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid触媒HCID 8857Ethyl Acetate溶媒

実験手順

N-aminophthalimide (476 mg) and 5N hydrochloric acid (5 drops) were added to the tetrahydrofuran solution (20 mL) of the compound prepared in Example 54 (1 g). The reaction mixture was stirred for 20 minutes under argon gas atmosphere. Ethyl acetate (100 mL) was added to the reaction mixture. The reaction mixture was washed by a saturated aqueous solution of sodium bicarbonate and a saturated aqueous solution of sodium chloride. The organic layer was dried with anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by column chromatography on silica gel (Yamazen corporation, high flash 2 L, n-hexane→ethyl acetate/n-hexane=1/4) to obtain the title compound (675 mg) having the following physical data.

後処理

  1. washThe reaction mixture was washed by a saturated aqueous solution of sodium bicarbonate
  2. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe obtained residue was purified by column chromatography on silica gel (Yamazen corporation, high flash 2 L, n-hexane→ethyl acetate/n-hexane=1/4)

出典と根拠

ORDレコード
ord-9256487772b84d7da862fb89310362a6
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08420810B2

反応ノート

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