Water → lithium 4-((2S,4R)-1-acetyl-2-methyl-4-(pyridin-2-ylamino)-1,2,3,4-tetrahydroquinolin-6-yl)benzoate

HRID 882258ノート

反応式

HRID 882258 の反応式
[C:1]([N:4]1[C:13]2[C:8](=[CH:9][C:10]([C:14]3[CH:24]=[CH:23][C:17]([C:18]([O:20]CC)=[O:19])=[CH:16][CH:15]=3)=[CH:11][CH:12]=2)[C@H:7]([NH:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][N:27]=2)[CH2:6][C@@H:5]1[CH3:32])(=[O:3])[CH3:2].O.O.[OH-].[Li+:36]>CCO>[C:1]([N:4]1[C:13]2[C:8](=[CH:9][C:10]([C:14]3[CH:24]=[CH:23][C:17]([C:18]([O-:20])=[O:19])=[CH:16][CH:15]=3)=[CH:11][CH:12]=2)[C@H:7]([NH:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][N:27]=2)[CH2:6][C@@H:5]1[CH3:32])(=[O:3])[CH3:2].[Li+:36]

参加物

5

反応物 3

HCID 962WaterHCID 168937Lithium hydroxide, monohydrate2 回HCID 86709426ethyl 4-((2S,4R)-1-acetyl-2-methyl-4-(pyridin-2-ylamino)-1,2,3,4-tetrahydroquinolin-6-yl)benzoate

生成物 1

HCID 70976493lithium 4-((2S,4R)-1-acetyl-2-methyl-4-(pyridin-2-ylamino)-1,2,3,4-tetrahydroquinolin-6-yl)benzoate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Ethyl 4-((2S,4R)-1-acetyl-2-methyl-4-(pyridin-2-ylamino)-1,2,3,4-tetrahydroquinolin-6-yl)benzoate (for a preparation see Intermediate 57) (216 mg, 0.503 mmol) in EtOH (1 mL) and water (0.5 mL) was treated with lithium hydroxide monohydrate (22 mg, 0.524 mmol) and the mixture stirred at r.t. over the weekend. A further portion of lithium hydroxide monohydrate (4 mg, 0.095 mmol) was added to the reaction and the mixture stirred for 1 h. The mixture was concentrated to dryness to give the crude product lithium 4-((2S,4R)-1-acetyl-2-methyl-4-(pyridin-2-ylamino)-1,2,3,4-tetrahydroquinolin-6-yl)benzoate (160 mg) which was used directly in the next step without further purification.

後処理

  1. stirringthe mixture stirred for 1 h
  2. concentrationThe mixture was concentrated to dryness

出典と根拠

ORDレコード
ord-131f290312714c2ab0187b5a7a93de60
出典データセット
uspto-grants-2015_03
特許番号
US08993554B2

反応ノート

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