HCID 86655023、化合物 → HCID 58333381、化合物

HRID 2066892ノート

反応式

HRID 2066892 の反応式
[F:1][C:2]1[CH:7]=[C:6]([S:8]([CH3:11])(=[O:10])=[O:9])[CH:5]=[CH:4][C:3]=1[N:12]1[CH2:17][CH2:16][C:15](=[N:18][O:19][CH:20]2[CH2:25][CH2:24][N:23]([C:26]#[N:27])[CH2:22][CH2:21]2)[CH2:14][CH2:13]1.[OH:28][NH:29][C:30](=N)[CH:31]([CH3:33])[CH3:32]>C(OCC)(=O)C.[Cl-].[Cl-].[Zn+2]>[CH:31]([C:30]1[N:27]=[C:26]([N:23]2[CH2:24][CH2:25][CH:20]([O:19][N:18]=[C:15]3[CH2:16][CH2:17][N:12]([C:3]4[CH:4]=[CH:5][C:6]([S:8]([CH3:11])(=[O:9])=[O:10])=[CH:7][C:2]=4[F:1])[CH2:13][CH2:14]3)[CH2:21][CH2:22]2)[O:28][N:29]=1)([CH3:33])[CH3:32]

参加物

5

反応物 2

HCID 86655023HCID 86655023、化合物HCID 178449908HCID 178449908、化合物

生成物 1

HCID 58333381HCID 58333381、化合物

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 8857Ethyl Acetate溶媒

実験手順

68b (35 mg, 0.066 mmol) and 68a (8 mg, 0.08 mmol) were combined in ethyl acetate (1 mL) and 1N ZnCl2 (80 μL, 0.08 mmol) was added dropwise. After 1 h, the solvent was evaporated. 1 mL of ethanol and 0.5 mL of concentrated HCl were added and the mixture was heated to reflux. The solvent was removed and the crude mixture was purified on preparative HPLC to give 68-1: LC-MS 480.2 (MH+), tR=5.57 (Method 5).

後処理

  1. customthe solvent was evaporated
  2. addition1 mL of ethanol and 0.5 mL of concentrated HCl were added
  3. temperaturethe mixture was heated to reflux
  4. customThe solvent was removed
  5. customthe crude mixture was purified on preparative HPLC
  6. customto give 68-1

出典と根拠

ORDレコード
ord-48cb117126574275b474e7ed042c68b9
出典データセット
uspto-grants-2012_10
特許番号
US08293729B2

反応ノート

読み込み中…