1,1'-Carbonyldiimidazole → HCID 59683283、化合物

HRID 2061490ノート

反応式

HRID 2061490 の反応式
[NH2:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([CH:9]2[CH2:11][CH2:10]2)=[CH:4][C:3]=1[NH:12][CH:13]1[CH2:18][CH2:17][N:16]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:15][CH2:14]1.C1N=CN([C:31](N2C=NC=C2)=[O:32])C=1>O1CCCC1>[CH:9]1([C:5]2[CH:6]=[C:7]([F:8])[C:2]3[NH:1][C:31](=[O:32])[N:12]([CH:13]4[CH2:18][CH2:17][N:16]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:15][CH2:14]4)[C:3]=3[CH:4]=2)[CH2:11][CH2:10]1

参加物

4

反応物 2

HCID 682631,1'-Carbonyldiimidazole2 回HCID 596832651,1-Dimethylethyl 4-[(2-amino-5-cyclopropyl-3-fluorophenyl)amino]-1-piperidinecarboxylate

生成物 1

HCID 59683283HCID 59683283、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1,1-Dimethylethyl 4-[(2-amino-5-cyclopropyl-3-fluorophenyl)amino]-1-piperidinecarboxylate (D27, 0.80 mmol, 280 mg) was dissolved in 4 ml of tetrahydrofuran and CDI (1,1′-(oxomethanediyl)bis-1H-imidazole) (2.5 eq., 2.0 mmol, 0.33 g) at room temperature and the mixture was stirred at 50° C. for one overnight under argon. Extra CDI (1 eq., 0.13 g, 0.80 mmol) was added and the mixture was refluxed for two extra hours. The mixture was cooled to room temperature and the solvent was evaporated to afford the crude compound which was purified by chromatography (ethyl acetate (50)-n-hexane (50)) to yield the title compound, 102 mg, 36%, M−−H=374.

後処理

  1. temperaturethe mixture was refluxed for two extra hours
  2. customthe solvent was evaporated
  3. customto afford the crude compound which
  4. customwas purified by chromatography (ethyl acetate (50)-n-hexane (50))

出典と根拠

ORDレコード
ord-ca384287b25c4c50913075b0b29165ea
出典データセット
uspto-grants-2012_10
特許番号
US08283364B2

反応ノート

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