Trifluoroacetic acid → HCID 89852058、化合物

HRID 627146ノート

反応式

HRID 627146 の反応式
[CH2:1]([O:4][N:5]([C@H:18]1[CH2:23][N:22](C(OC(C)(C)C)=O)[C@H:21]([CH2:31][O:32][CH3:33])[CH:20]=[C:19]1[C:34](=[O:36])[NH2:35])[S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[N+:15]([O-:17])=[O:16])(=[O:8])=[O:7])[CH:2]=[CH2:3].FC(F)(F)C(O)=O>ClCCl>[CH2:1]([O:4][N:5]([C@@H:18]1[C:19]([C:34]([NH2:35])=[O:36])=[CH:20][C@@H:21]([CH2:31][O:32][CH3:33])[NH:22][CH2:23]1)[S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[N+:15]([O-:17])=[O:16])(=[O:8])=[O:7])[CH:2]=[CH2:3]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 89863149(2S,5R)-tert-butyl 5-(N-(allyloxy)-2-nitrophenylsulfonamido)-4-carbamoyl-2-(methoxymethyl)-5,6-dihydropyridine-1(2H)-carboxylate

生成物 1

HCID 89852058HCID 89852058、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of Intermediate 112 (729 mg, 1.38 mmol) in dichloromethane (10 mL) was added trifluoroacetic acid (2133 μl, 27.69 mmol). This solution was slightly darker after addition. The reaction was placed under a nitrogen atmosphere and stirred until LCMS analysis indicated consumption of starting material (˜45 minutes). At that time, solvent was removed in vacuo. The residue was taken up in toluene and sonicated, and then toluene was removed in vacuo. This was repeated twice, affording an orange solid of high purity by proton NMR. The product was taken forward without further purification.

後処理

  1. additionafter addition
  2. customconsumption of starting material (˜45 minutes)
  3. customAt that time, solvent was removed in vacuo
  4. customsonicated
  5. customtoluene was removed in vacuo
  6. customaffording an orange solid of high purity by proton NMR
  7. customThe product was taken forward without further purification

出典と根拠

ORDレコード
ord-c91c1c4dcef440028f7e7a76c3efcb6c
出典データセット
uspto-grants-2016_04
特許番号
US09309245B2

反応ノート

読み込み中…