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Diisopropylethylamine → HCID 23550119, 화합물

HRID 1814703
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HRID 1814703 반응식
C(OC(=O)CCNC(=O)C1C=CC(CN)=CC=1)C.C1C2(CCCCC2)CCC(=O)C1.[CH2:31]([O:33][C:34](=[O:59])[CH2:35][CH2:36][NH:37][C:38](=[O:58])[C:39]1[CH:44]=[CH:43][C:42]([CH2:45][NH:46][CH:47]2[CH2:52][CH2:51][C:50]3([CH2:57][CH2:56][CH2:55][CH2:54][CH2:53]3)[CH2:49][CH2:48]2)=[CH:41][CH:40]=1)[CH3:32].C(N(C(C)C)CC)(C)C.[F:69][C:70]1[CH:71]=[C:72]([CH:76]=[C:77]([C:79]([F:82])([F:81])[F:80])[CH:78]=1)[C:73](Cl)=[O:74]>C(#N)C>[CH2:31]([O:33][C:34](=[O:59])[CH2:35][CH2:36][NH:37][C:38](=[O:58])[C:39]1[CH:44]=[CH:43][C:42]([CH2:45][NH:46][CH:47]2[CH2:52][CH2:51][C:50]3([CH2:53][CH2:54][CH2:55][CH2:56][CH2:57]3)[CH2:49][CH2:48]2)=[CH:41][CH:40]=1)[CH3:32].[CH2:31]([O:33][C:34](=[O:59])[CH2:35][CH2:36][NH:37][C:38](=[O:58])[C:39]1[CH:44]=[CH:43][C:42]([CH2:45][N:46]([C:73](=[O:74])[C:72]2[CH:76]=[C:77]([C:79]([F:80])([F:81])[F:82])[CH:78]=[C:70]([F:69])[CH:71]=2)[CH:47]2[CH2:52][CH2:51][C:50]3([CH2:53][CH2:54][CH2:55][CH2:56][CH2:57]3)[CH2:49][CH2:48]2)=[CH:41][CH:40]=1)[CH3:32]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 81531DiisopropylethylamineHCID 5193643-Fluoro-5-(trifluoromethyl)benzoyl chlorideHCID 574172Spiro[5.5]undecan-3-oneHCID 22502126HCID 22502126, 화합물HCID 23550130HCID 23550130, 화합물

생성물 2

HCID 23550119HCID 23550119, 화합물수율 200.2%
HCID 23550130
HCID 23550130, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

3-[4-(Spiro[5.5]undec-3-ylaminomethyl)benzoylamino]propionic acid ethyl ester was prepared by reductive alkylation of 3-(4-aminomethyl-benzoylamino)propionic acid ethyl ester with spiro[5.5]undecan-3-one. 3-[4-(Spiro[5.5]undec-3-ylaminomethyl)benzoylamino]propionic acid ethyl ester (200 mg, 499 μmol) was dissolved in acetonitrile (5 mL) and diisopropylethylamine (170 μL) and cooled on an ice bath. Commercially available 3-fluoro-5-(trifluoromethyl)benzoylchloride (136 mg, 602 μmol) dissolved in acetonitrile (5 mL) was added dropwise. The reaction was complete within one hour as shown by HPLC. The solvent was evaporated and water (10 mL) was added to the residue followed by saturated sodium bicarbonate (10 mL). The product was extracted using ethyl acetate (2×50 mL). The combined ethyl acetate extracts were washed with water (20 mL) and brine (20 mL). Drying the organic phases over MgSO4 and evaporation of the solvent afforded 3-(4-{[(3-fluoro-5-trifluoromethylbenzoyl)spiro[5.5]undec-3-yl-amino]methyl}benzoylamino)propionic acid ethyl ester (295 mg) which was hydrolyzed using sodium hydroxide to afford the title compound.

후처리

  1. additionwas added dropwise
  2. customThe solvent was evaporated
  3. additionwater (10 mL) was added to the residue
  4. extractionThe product was extracted
  5. washThe combined ethyl acetate extracts were washed with water (20 mL) and brine (20 mL)
  6. customDrying the organic phases
  7. customover MgSO4 and evaporation of the solvent

출처 및 근거

ORD 기록
ord-351041bc342047979ad8ef5cf357ab37
출처 데이터셋
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06875760B2

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