Water → 10-[1,4]Oxazepan-4-yl-5,6,8,9-tetrahydro-1,4,7,10a-tetraaza-cyclohepta[f]indene-7-carboxylic acid tert-butyl ester

HRID 528710노트

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HRID 528710 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:22][CH2:21][C:12]2=[C:13](Cl)[N:14]3[C:18]([N:19]=[C:11]2[CH2:10][CH2:9]1)=[CH:17][CH:16]=[N:15]3)=[O:7])([CH3:4])([CH3:3])[CH3:2].CCN(C(C)C)C(C)C.[CH2:32]1[CH2:38][O:37][CH2:36][CH2:35][NH:34][CH2:33]1.Cl.O>C(O)C>[C:1]([O:5][C:6]([N:8]1[CH2:22][CH2:21][C:12]2=[C:13]([N:34]3[CH2:33][CH2:32][CH2:38][O:37][CH2:36][CH2:35]3)[N:14]3[C:18]([N:19]=[C:11]2[CH2:10][CH2:9]1)=[CH:17][CH:16]=[N:15]3)=[O:7])([CH3:4])([CH3:3])[CH3:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 230902141,4-Oxazepane hydrochlorideHCID 4692812210-Chloro-5,6,8,9-tetrahydro-1,4,7,10a-tetraaza-cyclohepta[f]indene-7-carboxylic acid tert-butyl ester

생성물 1

HCID 6797938810-[1,4]Oxazepan-4-yl-5,6,8,9-tetrahydro-1,4,7,10a-tetraaza-cyclohepta[f]indene-7-carboxylic acid tert-butyl ester

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
80 °C

실험 절차

To 0.1 g (0.31 mmol) 10-chloro-5,6,8,9-tetrahydro-1,4,7,10a-tetraaza-cyclohepta[f]indene-7-carboxylic acid tert-butyl ester, in a sealed tube in 4 mL ethanol, was added 0.2 mL (1.12 mmol) DIPEA followed by 47 mg (0.34 mmol) homomorpholine hydrochloride, and the reaction was heated at 80° C. for 16 hours. 5 mL of H2O was added and the mixture was extracted with EtOAc (2×10 mL), the organic layers were combined and dried with MgSO4. After filtration and evaporation of the solvent the product was purified by column chromatography (silica, hexane/EtOAc 10:0 to 6:4).

후처리

  1. extractionthe mixture was extracted with EtOAc (2×10 mL)
  2. dry with materialdried with MgSO4
  3. filtrationAfter filtration and evaporation of the solvent the product
  4. customwas purified by column chromatography (silica, hexane/EtOAc 10:0 to 6:4)

출처 및 근거

ORD 기록
ord-91941adcc2cf4feb9af1690e9ca54ee8
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346816B2

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