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Diisopropylethylamine → HCID 67355233, 화합물

HRID 627391
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HRID 627391 반응식
[CH:1]1([N:7]2[C:11]3[N:12]=[C:13]([NH:16][C:17]4[CH:25]=[CH:24][C:20]([C:21](O)=[O:22])=[CH:19][N:18]=4)[N:14]=[CH:15][C:10]=3[CH:9]=[C:8]2[C:26](=[O:30])[N:27]([CH3:29])[CH3:28])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.CCN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[C:64]([O:68][C:69]([N:71]1[CH:76]2[CH2:77][CH2:78][CH:72]1[CH2:73][NH:74][CH2:75]2)=[O:70])([CH3:67])([CH3:66])[CH3:65]>CN(C=O)C>[C:64]([O:68][C:69]([N:71]1[CH:72]2[CH2:78][CH2:77][CH:76]1[CH2:75][N:74]([C:21]([C:20]1[CH:19]=[N:18][C:17]([NH:16][C:13]3[N:14]=[CH:15][C:10]4[CH:9]=[C:8]([C:26](=[O:30])[N:27]([CH3:29])[CH3:28])[N:7]([CH:1]5[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]5)[C:11]=4[N:12]=3)=[CH:25][CH:24]=1)=[O:22])[CH2:73]2)=[O:70])([CH3:67])([CH3:65])[CH3:66]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 157409088-Boc-3,8-diaza-bicyclo(3.2.1)octaneHCID 67354845HCID 67354845, 화합물

생성물 1

HCID 67355233HCID 67355233, 화합물수율 82%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a 1 mL DMF solution of 6-(7-cyclohexyl-6-dimethylcarbamoyl-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino)-nicotinic acid (50 mg, 0.122 mmol) was added DIPEA (32 mg, 0.043 mmol) and HBTU (49 mg, 0.129 mmol). After stirring for 15 m at room temperature 3,8-diaza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester (31.2 mg, 0.147 mmol) was added and the reaction mixture was left to stir at room temperature for 4 h. The reaction was quenched by pouring into brine and extracted with EtOAc. The organic extracts were dried with Na2SO4, filtered and concentrated. The crude product was purified by NP-LC (Analogix, 10% MeOH in EtOAc) to yield 3-[6-(7-cyclohexyl-6-dimethylcarbamoyl-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino)-pyridine-3-carbonyl]-3,8-diaza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester (60 mg, 0.10 mmol). MS m/z 603.5 (M+H)+.

후처리

  1. additionwas added
  2. waitthe reaction mixture was left
  3. customThe reaction was quenched
  4. additionby pouring into brine
  5. extractionextracted with EtOAc
  6. dry with materialThe organic extracts were dried with Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe crude product was purified by NP-LC (Analogix, 10% MeOH in EtOAc)

출처 및 근거

ORD 기록
ord-0868de36093d47f3a7e94c5e0ae79c11
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09309252B2

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