Diisopropylethylamine → HCID 67457877, 화합물

HRID 528771노트

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HRID 528771 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].[NH:23]1[CH2:26][CH:25]([CH2:27][C:28]([OH:30])=[O:29])[CH2:24]1.CCN(C(C)C)C(C)C>C(O)C>[C:1]([O:5][C:6]([N:8]1[CH2:22][CH2:21][C:12]2=[C:13]([N:23]3[CH2:26][CH:25]([CH2:27][C:28]([OH:30])=[O:29])[CH2:24]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

5

반응물 3

HCID 81531DiisopropylethylamineHCID 117685473-Azetidineacetic acidHCID 4692812210-Chloro-5,6,8,9-tetrahydro-1,4,7,10a-tetraaza-cyclohepta[f]indene-7-carboxylic acid tert-butyl ester

생성물 1

HCID 67457877HCID 67457877, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
75 °C

실험 절차

2.5 g (7.75 mmol) 10-Chloro-5,6,8,9-tetrahydro-1,4,7,10a-tetraaza-cyclohepta[f]indene-7-carboxylic acid tert-butyl ester, 1.1 g (9.1 mmol) azetidin-3-yl-acetic acid and 3 mL (17.4 mmol) DIPEA were suspended in 18 mL ethanol. The reaction mixture was stirred at 75° C. over night. The solvent was evaporated and the residue was taken up in EtOAc and water and was acidified using a KHSO4 solution. The organic layer was dried (Na2SO4) and concentrated. The residue was purified by prep. HPLC to yield the corresponding acid (72% of theory).

후처리

  1. customThe solvent was evaporated
  2. dry with materialThe organic layer was dried (Na2SO4)
  3. concentrationconcentrated
  4. customThe residue was purified by prep
  5. customHPLC to yield the corresponding acid (72% of theory)

출처 및 근거

ORD 기록
ord-082f5df909f9427f851eee7480327657
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346816B2

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