Trifluoroacetic acid → HCID 91665637、化合物

HRID 1035321ノート

反応式

HRID 1035321 の反応式
[CH2:1]([N:8]([CH2:25][C:26]([O:28]CC)=O)[C:9](=[O:24])[C@H:10]([NH:16]C(OC(C)(C)C)=O)[CH2:11][C:12]([O:14][CH3:15])=[O:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.F[C:32](F)(F)C(O)=O>ClCCl>[CH2:1]([N:8]1[CH2:25][C:26](=[O:28])[NH:16][C@H:10]([CH2:11][C:12]([O:14][CH2:15][CH3:32])=[O:13])[C:9]1=[O:24])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 67248809HCID 67248809、化合物

生成物 1

HCID 91665637HCID 91665637、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
70 °C

実験手順

To a solution of Example 255C (50.75 g, 120 mmol) in dichloromethane (50 mL) was added trifluoroacetic acid. The reaction was stirred overnight and then concentrated. Ammonia was added (7 N, methanol, 250 mL) and the solution was warmed to 70° C. for 2 hours. The reaction was concentrated and dichloromethane was added (500 mL). The solution stirred for 10 minutes before the salt was removed by filtration. The solution was then concentrated and purification via flash chromatography (3% 2 N NH3 in methanol/dichloromethane) afforded the title compound.

後処理

  1. concentrationconcentrated
  2. additionAmmonia was added (7 N, methanol, 250 mL)
  3. concentrationThe reaction was concentrated
  4. additiondichloromethane was added (500 mL)
  5. stirringThe solution stirred for 10 minutes before the salt
  6. customwas removed by filtration
  7. concentrationThe solution was then concentrated
  8. custompurification via flash chromatography (3% 2 N NH3 in methanol/dichloromethane)

出典と根拠

ORDレコード
ord-eaff4d23406047628cb7089bb2a458f0
出典データセット
uspto-grants-2013_10
特許番号
US08546377B2

反応ノート

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