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Water → N-[2-[2-[(1,1-dimethylethyl)amino]ethoxy]phenyl]-1H-indol-4-carboxamide

HRID 1091129
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HRID 1091129 반응식
Cl[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[NH:11][C:12]([C:14]1[C:15]2[CH:16]=[CH:17][NH:18][C:19]=2[CH:20]=[CH:21][CH:22]=1)=[O:13].O.[OH-].[Na+].C(=O)([O-])[O-].[K+].[K+].[C:32]([NH2:36])([CH3:35])([CH3:34])[CH3:33]>C(O)C.C(OCC)(=O)C>[CH3:33][C:32]([NH:36][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[NH:11][C:12]([C:14]1[C:15]2[CH:16]=[CH:17][NH:18][C:19]=2[CH:20]=[CH:21][CH:22]=1)=[O:13])([CH3:35])[CH3:34]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 962WaterHCID 6385Tert-ButylamineHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 13787419N-[2-(2-chloroethoxy)phenyl]-1H-indol-4-carboxamide

생성물 1

HCID 3086996N-[2-[2-[(1,1-dimethylethyl)amino]ethoxy]phenyl]-1H-indol-4-carboxamide

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

With stirring at a pressure of 2 bars, a solution of 2.3 g of the product from Step A in 40 ml of ethanol and 37.5 ml of tert-butylamine was heated at 120° C. for 24 hours. After dilution with 400 ml of water and 400 ml of ethyl acetate, the solution was alkalized with sodium hydroxide and saturated with potassium carbonate. The mixture was extracted with ethyl acetate and the crystals obtained were triturated with ether to obtain 2.3 g of N-[2-[2-[(1,1-dimethylethyl)amino]ethoxy]phenyl]-1H-indol-4-carboxamide melting at ≃148° C.

후처리

  1. extractionThe mixture was extracted with ethyl acetate
  2. customthe crystals obtained
  3. customwere triturated with ether

출처 및 근거

ORD 기록
ord-b495cc0cc22940b4ab77793684e69227
출처 데이터셋
uspto-grants-1992_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05084455

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