Hydrochloric Acid → [7-Chloro-1-isobutyl-5-(2-methoxyphenyl)-2-oxo-1,2,4,5-tetrahydro-3H-3-benzazepin-3-yl]acetic acid

HRID 1444835

반응식

HRID 1444835 반응식
C([O:3][C:4](=[O:31])[CH2:5][N:6]1[C:12](=[O:13])[CH:11]([CH2:14][CH:15]([CH3:17])[CH3:16])[C:10]2[CH:18]=[CH:19][C:20]([Cl:22])=[CH:21][C:9]=2[CH:8]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[O:29][CH3:30])[CH2:7]1)C.[OH-].[Na+].Cl>O1CCOCC1.O>[Cl:22][C:20]1[CH:19]=[CH:18][C:10]2[CH:11]([CH2:14][CH:15]([CH3:16])[CH3:17])[C:12](=[O:13])[N:6]([CH2:5][C:4]([OH:31])=[O:3])[CH2:7][CH:8]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[O:29][CH3:30])[C:9]=2[CH:21]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 59025486Ethyl[7-chloro-1-isobutyl-5-(2-methoxyphenyl)-2-oxo-1,2,4,5-tetrahydro-3H-3-benzazepin-3-yl]-acetate

생성물 1

HCID 59025496[7-Chloro-1-isobutyl-5-(2-methoxyphenyl)-2-oxo-1,2,4,5-tetrahydro-3H-3-benzazepin-3-yl]acetic acid

시약·촉매·용매 1

HCID 218864351,4-Dioxane--water (1/1)용매

실험 절차

85 mg of the compound from Example 23A (0.19 mol) are dissolved in 3.5 ml of dioxane/water (1:1) and mixed with 0.29 ml of 1 N sodium hydroxide solution (0.29 mol). The reaction mixture is stirred at room temperature for 3 h. It is acidified with 5 ml of 1 N hydrochloric acid, and the mixture is extracted three times with dichloromethane. The combined organic phases are dried over sodium sulphate and concentrated in a rotary evaporator. 80 mg (100% of theory) of the title compound are obtained.

후처리

  1. extractionthe mixture is extracted three times with dichloromethane
  2. dry with materialThe combined organic phases are dried over sodium sulphate
  3. concentrationconcentrated in a rotary evaporator

출처 및 근거

ORD 기록
ord-2a0f609edf0247f3ba13bf67cf440757
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07662956B2

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