2-Pentanamine → (2-{[5-(1-Methyl-butylcarbamoyl)-thiophene-2-carbonyl]-amino}-phenyl)-carbamic acid tert-butyl ester

HRID 1790216ノート

反応式

HRID 1790216 の反応式
[C:1]([O:5][C:6]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[NH:15][C:16]([C:18]1[S:22][C:21]([C:23]([OH:25])=O)=[CH:20][CH:19]=1)=[O:17])=[O:7])([CH3:4])([CH3:3])[CH3:2].C(N1C=CN=C1)(N1C=CN=C1)=O.[CH3:38][CH:39]([NH2:43])[CH2:40][CH2:41][CH3:42]>C1COCC1>[C:1]([O:5][C:6](=[O:7])[NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[NH:15][C:16]([C:18]1[S:22][C:21]([C:23](=[O:25])[NH:43][CH:39]([CH3:38])[CH2:40][CH2:41][CH3:42])=[CH:20][CH:19]=1)=[O:17])([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 122462-PentanamineHCID 682631,1'-CarbonyldiimidazoleHCID 58191955HCID 58191955、化合物

生成物 1

HCID 69055708(2-{[5-(1-Methyl-butylcarbamoyl)-thiophene-2-carbonyl]-amino}-phenyl)-carbamic acid tert-butyl ester

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
45 °C

実験手順

To a solution of 4.4 g (12.1 mmol) 5-(2-tert-butoxycarbonylamino-phenylcarbamoyl)-thiophene-2-carboxylic acid in 80 ml THF were added 2.2 g (13.6 mmol) carbonyldiimidazol. The reaction mixture was stirred at 45° C. for 1 h and then cooled to rt. After addition of 1.05 g (12 mmol) 2-pentylamine the reaction mixture was kept at rt for 12 h. The solvent was evaporated and the residue was dissolved in 150 ml CH2 Cl2. The solution was washed twice with 150 ml water each and dried over magnesium sulfate. The solvent was evaporated and the residue was washed with diethyl ether to yield (2-{[5-(1-methyl-butylcarbamoyl)-thiophene-2-carbonyl]-amino}-phenyl)-carbamic acid tert-butyl ester as a white solid, mp. 183° C.

後処理

  1. temperaturecooled to rt
  2. waitwas kept at rt for 12 h
  3. customThe solvent was evaporated
  4. dissolutionthe residue was dissolved in 150 ml CH2 Cl2
  5. washThe solution was washed twice with 150 ml water each and
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent was evaporated
  8. washthe residue was washed with diethyl ether

出典と根拠

ORDレコード
ord-a2cea9a32b0044a881f3c9217467f865
出典データセット
uspto-grants-2006_07
特許番号
US07071219B2

反応ノート

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