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Sodium Carbonate → (S)-2-(2-aminophenyl)-7-methoxy-8-(3-(((S)-7-methoxy-2-(4-methoxyphenyl)-5,11-dioxo-10((2-(trimethylsilyl)ethoxy)methyl)-5,10,11,11a-tetrahydro-pyrrolo[2,1-c][1,4]benzodiazepin-8-yl)oxy)propoxy)-10-((2-(trimethylsilyl)ethoxy)methyl)-pyrrolo[2,1-c][1,4]-benzodiazepine-5,11(10H,11aH)-dione

HRID 594185
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인쇄 미리보기

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HRID 594185 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH2:10][C@@H:11]3[N:17]([CH:18]=2)[C:16](=[O:19])[C:15]2[CH:20]=[C:21]([O:62][CH3:63])[C:22]([O:24][CH2:25][CH2:26][CH2:27][O:28][C:29]4[C:59]([O:60][CH3:61])=[CH:58][C:32]5[C:33](=[O:57])[N:34]6[CH:49]=[C:48](S(C(F)(F)F)(=O)=O)[CH2:47][C@H:35]6[C:36](=[O:46])[N:37]([CH2:38][O:39][CH2:40][CH2:41][Si:42]([CH3:45])([CH3:44])[CH3:43])[C:31]=5[CH:30]=4)=[CH:23][C:14]=2[N:13]([CH2:64][O:65][CH2:66][CH2:67][Si:68]([CH3:71])([CH3:70])[CH3:69])[C:12]3=[O:72])=[CH:5][CH:4]=1.[NH2:73][C:74]1[CH:79]=[CH:78][CH:77]=[CH:76][C:75]=1B(O)O.C(=O)([O-])[O-].[Na+].[Na+].C(OCC)(=O)C.CCCCCC>C(O)C.C1(C)C=CC=CC=1.O.C(OCC)(=O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[NH2:73][C:74]1[CH:79]=[CH:78][CH:77]=[CH:76][C:75]=1[C:48]1[CH2:47][C@@H:35]2[N:34]([CH:49]=1)[C:33](=[O:57])[C:32]1[CH:58]=[C:59]([O:60][CH3:61])[C:29]([O:28][CH2:27][CH2:26][CH2:25][O:24][C:22]3[C:21]([O:62][CH3:63])=[CH:20][C:15]4[C:16](=[O:19])[N:17]5[CH:18]=[C:9]([C:6]6[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:8][CH:7]=6)[CH2:10][C@H:11]5[C:12](=[O:72])[N:13]([CH2:64][O:65][CH2:66][CH2:67][Si:68]([CH3:69])([CH3:71])[CH3:70])[C:14]=4[CH:23]=3)=[CH:30][C:31]=1[N:37]([CH2:38][O:39][CH2:40][CH2:41][Si:42]([CH3:43])([CH3:44])[CH3:45])[C:36]2=[O:46]
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참가 물질

10

반응물 4

HCID 10340Sodium CarbonateHCID 2773216(2-Aminophenyl)boronic acidHCID 21226206Ethyl acetate hexaneHCID 86676188HCID 86676188, 화합물

생성물 1

HCID 86676192
(S)-2-(2-aminophenyl)-7-methoxy-8-(3-(((S)-7-methoxy-2-(4-methoxyphenyl)-5,11-dioxo-10((2-(trimethylsilyl)ethoxy)methyl)-5,10,11,11a-tetrahydro-pyrrolo[2,1-c][1,4]benzodiazepin-8-yl)oxy)propoxy)-10-((2-(trimethylsilyl)ethoxy)methyl)-pyrrolo[2,1-c][1,4]-benzodiazepine-5,11(10H,11aH)-dione
수율 90.3%

시약·촉매·용매 5

HCID 178418397HCID 178418397, 화합물촉매HCID 702Ethanol용매HCID 962Water용매HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

반응 조건

온도
40 °C

실험 절차

A catalytic amount of tetrakistriphenylphosphinepalladium (0) (11.2 mg) was added to a mixture of the mono triflate 17 (380 mg), the pinnacol ester of 2-aminophenylboronic acid (124 mg) and sodium carbonate (120 mg) in ethanol (5 mL), toluene (5 mL) and water (5 mL). The reaction mixture was allowed to stir over night at room temperature and at 40° C. until the reaction was complete (c. 2 hr). The reaction mixture was diluted with ethyl acetate and the organic layer was washed with water and brine. The ethyl acetate solution was dried over magnesium sulphate and filtered under vacuum. Removal of ethyl acetate by rotary evaporation under reduced pressure afforded the crude product which was subjected to flash chromatography (silica gel, ethyl acetate/hexane). Pure fractions were collected and combined. Removal of excess eluent by rotary evaporation under reduced pressure afforded the pure product 103 (330 mg, 86% yield). LC/MS RT: 4.17 min, ES+1018.48.

후처리

  1. custom(c. 2 hr)
  2. washthe organic layer was washed with water and brine
  3. dry with materialThe ethyl acetate solution was dried over magnesium sulphate
  4. filtrationfiltered under vacuum
  5. customRemoval of ethyl acetate
  6. customby rotary evaporation under reduced pressure
  7. customafforded the crude product which
  8. customPure fractions were collected
  9. customRemoval of excess eluent
  10. customby rotary evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-a92c967aabcf4731b4bdbaf5618861cb
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09242013B2

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