Sodium Hydroxide → HCID 59703554、化合物

HRID 556474ノート

反応式

HRID 556474 の反応式
C[O:2][C:3]([CH:5]1[CH2:13][C:12]2[C:7](=[CH:8][C:9]([O:14][CH3:15])=[CH:10][CH:11]=2)[N:6]1[C:16]1([CH2:27][C:28]2[CH:33]=[CH:32][CH:31]=[C:30]([Cl:34])[CH:29]=2)[C:24]2[C:19](=[CH:20][C:21]([Cl:25])=[CH:22][CH:23]=2)[NH:18][C:17]1=[O:26])=[O:4].[OH-].[Na+]>CO.O>[Cl:25][C:21]1[CH:20]=[C:19]2[C:24]([C:16]([CH2:27][C:28]3[CH:33]=[CH:32][CH:31]=[C:30]([Cl:34])[CH:29]=3)([N:6]3[C:7]4[C:12](=[CH:11][CH:10]=[C:9]([O:14][CH3:15])[CH:8]=4)[CH2:13][CH:5]3[C:3]([OH:4])=[O:2])[C:17](=[O:26])[NH:18]2)=[CH:23][CH:22]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 66992271Rac-6'-chloro-3'-(3-chloro-benzyl)-6-methoxy-2'-oxo-2,3,2',3'-tetrahydro-1'h-[1,3']biindolyl-2-carboxylic acid methyl ester

生成物 1

HCID 59703554HCID 59703554、化合物収率 103.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

A mixture of rac-6′-Chloro-3′-(3-chloro-benzyl)-6-methoxy-2′-oxo-2,3,2′,3′-tetrahydro-1′H-[1,3′]biindolyl-2-carboxylic acid methyl ester (250 mg, 0.5 mmol), NaOH (40 mg, 1.0 mmol) in methanol (4 mL) and water (2 mL) was heated to reflux for 3 hr. Then the mixture was concentrated in vacuo to remove methanol. Water (10 mL) was added to the residue. The resulting mixture was acidified with acetic acid, extracted with ethyl acetate. The organic layer was washed with water, dried with Na2SO4, concentrated in vacuo to give 250 mg rac-6′-Chloro-3′-(3-chloro-benzyl)-6-methoxy-2′-oxo-2,3,2′,3′-tetrahydro-1′H-[1,3′]biindolyl-2-carboxylic acid. MS: [M−H]−=481

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 3 hr
  3. concentrationThen the mixture was concentrated in vacuo
  4. customto remove methanol
  5. additionWater (10 mL) was added to the residue
  6. extractionextracted with ethyl acetate
  7. washThe organic layer was washed with water
  8. dry with materialdried with Na2SO4
  9. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c771ae2a6cfa41a89e6c52be26b7ef20
出典データセット
uspto-grants-2011_11
特許番号
US08058269B2

反応ノート

読み込み中…