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

HRID 882258노트

반응식

HRID 882258 반응식
[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]

참가 물질

5

반응물 3

HCID 962WaterHCID 168937Lithium hydroxide, monohydrate2회HCID 86709426ethyl 4-((2S,4R)-1-acetyl-2-methyl-4-(pyridin-2-ylamino)-1,2,3,4-tetrahydroquinolin-6-yl)benzoate

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-131f290312714c2ab0187b5a7a93de60
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08993554B2

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