Sodium Hydroxide → HCID 178445683、化合物

HRID 1992802ノート

反応式

HRID 1992802 の反応式
[C:1]([C@@H:5]1[CH2:10][CH2:9][C@H:8]([NH:11][C:12]([C:14]2[N:18]([CH2:19][C:20]3[CH:29]=[CH:28][C:23]([C:24]([O:26]C)=[O:25])=[CH:22][N:21]=3)[N:17]=[C:16]([C:30]3[CH:35]=[CH:34][C:33]([Cl:36])=[C:32]([Cl:37])[CH:31]=3)[CH:15]=2)=[O:13])[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+]>C1COCC1.CO>[C:1]([C@@H:5]1[CH2:6][CH2:7][C@H:8]([NH:11][C:12]([C:14]2[N:18]([CH2:19][C:20]3[CH:29]=[CH:28][C:23]([C:24]([OH:26])=[O:25])=[CH:22][N:21]=3)[N:17]=[C:16]([C:30]3[CH:35]=[CH:34][C:33]([Cl:36])=[C:32]([Cl:37])[CH:31]=3)[CH:15]=2)=[O:13])[CH2:9][CH2:10]1)([CH3:4])([CH3:2])[CH3:3]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 178497906HCID 178497906、化合物

生成物 1

HCID 178445683HCID 178445683、化合物

試薬・触媒・溶媒 1

HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

To a solution of the intermediate from step G (isomer B) (0.14 g, 0.24 mmol) in 10 ml of 1:1 THF/MeOH was added 5 N NaOH (1 mL). After stirring the reaction at room temperature for 2 hours, it was concentrated in vacuo. The residue was acidified with 1N HCl (10 ml) and the resulting mixture was extracted with ethyl acetate, dried over anhydrous Na2SO4 filtered and concentrated in vacuo. This material was used in the next step without any further purification.

後処理

  1. customthe reaction at room temperature for 2 hours
  2. concentrationit was concentrated in vacuo
  3. extractionthe resulting mixture was extracted with ethyl acetate
  4. dry with materialdried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThis material was used in the next step without any further purification

出典と根拠

ORDレコード
ord-df8d3c8f27c5484386299df76527078d
出典データセット
uspto-grants-2010_01
特許番号
US07649009B2

反応ノート

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