Phthalimide → HCID 66720712、化合物

HRID 1639767ノート

反応式

HRID 1639767 の反応式
[CH3:1][N:2]1[CH:10]=[C:9]2[C:4]([CH:5]=[CH:6][CH:7]=[C:8]2[C@H:11]2[CH2:13][C@H:12]2[CH2:14]O)=[N:3]1.N(C(OCC)=O)=NC(OCC)=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:47]1(=[O:57])[NH:51][C:50](=[O:52])[C:49]2=[CH:53][CH:54]=[CH:55][CH:56]=[C:48]12>O1CCCC1.C1(C)C=CC=CC=1>[CH3:1][N:2]1[CH:10]=[C:9]2[C:4]([CH:5]=[CH:6][CH:7]=[C:8]2[C@H:11]2[CH2:13][C@H:12]2[CH2:14][N:51]2[C:47](=[O:57])[C:48]3[C:49](=[CH:53][CH:54]=[CH:55][CH:56]=3)[C:50]2=[O:52])=[N:3]1

参加物

7

反応物 4

HCID 6809Phthalimide2 回HCID 11776Triphenylphosphine2 回HCID 220568ethyl N-ethoxycarbonyliminocarbamate2 回HCID 66720670cis-[2-(2-methyl-2H-indazol-4-yl)cyclopropyl]methanol

生成物 1

HCID 66720712HCID 66720712、化合物

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

Under argon gas atmosphere, to a solution of cis-[2-(2-methyl-2H-indazol-4-yl)cyclopropyl]methanol (130 mg, 0.643 mmol) in tetrahydrofuran (6.5 mL) were added a solution (40%, 0.351 mL, 0.771 mmol) of diethyl azodicarboxylate in toluene, triphenylphosphine (219 mg, 0.835 mmol) and phthalimide (123 mg, 0.836 mmol), and the mixture was stirred at room temperature for 5 hr. To the reaction mixture was added a solution (40%, 0.176 mL, 0.386 mmol) of diethyl azodicarboxylate in toluene, triphenylphosphine (110 mg, 0.419 mmol) and phthalimide (61.5 mg, 0.418 mmol) were added, and the mixture was stirred at room temperature for 30 min. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane=20/80→50/50) to give the title compound as a crudely purified product.

後処理

  1. additionwere added
  2. stirringthe mixture was stirred at room temperature for 30 min
  3. customThe solvent was evaporated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane=20/80→50/50)

出典と根拠

ORDレコード
ord-ab183daf25ff4819b3d72df0ba55d753
出典データセット
uspto-grants-2012_02
特許番号
US08110585B2

反応ノート

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