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Sodium Carbonate → HCID 86676191, 화합물

HRID 1429674
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HRID 1429674 반응식
Cl.[NH2:2][CH2:3][C:4]1[CH:9]=[CH:8][C:7](B(O)O)=[CH:6][CH:5]=1.[CH3:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]2[CH2:22][C@@H:23]3[N:29]([CH:30]=2)[C:28](=[O:31])[C:27]2[CH:32]=[C:33]([O:74][CH3:75])[C:34]([O:36][CH2:37][CH2:38][CH2:39][O:40][C:41]4[C:71]([O:72][CH3:73])=[CH:70][C:44]5[C:45](=[O:69])[N:46]6[CH:61]=[C:60](S(C(F)(F)F)(=O)=O)[CH2:59][C@H:47]6[C:48](=[O:58])[N:49]([CH2:50][O:51][CH2:52][CH2:53][Si:54]([CH3:57])([CH3:56])[CH3:55])[C:43]=5[CH:42]=4)=[CH:35][C:26]=2[N:25]([CH2:76][O:77][CH2:78][CH2:79][Si:80]([CH3:83])([CH3:82])[CH3:81])[C:24]3=[O:84])=[CH:17][CH:16]=1.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1.C(O)C.O>[NH2:2][CH2:3][C:4]1[CH:9]=[CH:8][C:7]([C:60]2[CH2:59][C@@H:47]3[N:46]([CH:61]=2)[C:45](=[O:69])[C:44]2[CH:70]=[C:71]([O:72][CH3:73])[C:41]([O:40][CH2:39][CH2:38][CH2:37][O:36][C:34]4[C:33]([O:74][CH3:75])=[CH:32][C:27]5[C:28](=[O:31])[N:29]6[CH:30]=[C:21]([C:18]7[CH:17]=[CH:16][C:15]([O:14][CH3:13])=[CH:20][CH:19]=7)[CH2:22][C@H:23]6[C:24](=[O:84])[N:25]([CH2:76][O:77][CH2:78][CH2:79][Si:80]([CH3:81])([CH3:82])[CH3:83])[C:26]=5[CH:35]=4)=[CH:42][C:43]=2[N:49]([CH2:50][O:51][CH2:52][CH2:53][Si:54]([CH3:57])([CH3:56])[CH3:55])[C:48]3=[O:58])=[CH:6][CH:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 10340Sodium CarbonateHCID 27343114-(Aminomethyl)benzeneboronic acid hydrochlorideHCID 86676188HCID 86676188, 화합물

생성물 1

HCID 86676191HCID 86676191, 화합물수율 61%

시약·촉매·용매 3

HCID 702Ethanol용매
HCID 962
Water
용매
HCID 1140Toluene용매

반응 조건

온도
30 °C

실험 절차

Solid 4-aminomethylbenzeneboronic acid hydrochloride (0.111 g, 0.59 mmol) was added to a solution of 17 (0.394 g, 0.37 mmol), sodium carbonate (175 mg, 1.654 mmol) and palladium tetrakis triphenylphosphine (28.0 mg, 0.024 mmol) in toluene (10 mL), ethanol (5 mL) and water (5 mL). The reaction mixture was allowed to stir overnight at 30° C. The following day the reaction mixture was heated for a further 3 hours at 70° C. The reaction mixture was then partitioned between ethyl acetate and water. The organic layer was washed with water and brine and dried over magnesium sulphate. Excess solvent was removed by rotary evaporation under reduced pressure and the resulting residue was subjected to flash column chromatography (silica gel; gradient elution EtOAc/hexane 2/9815/85). Removal of excess eluent from selected fractions afforded the desired product (0.230 mg, 0.22 mmol, 61%).

후처리

  1. temperatureThe following day the reaction mixture was heated for a further 3 hours at 70° C
  2. customThe reaction mixture was then partitioned between ethyl acetate and water
  3. washThe organic layer was washed with water and brine
  4. dry with materialdried over magnesium sulphate
  5. customExcess solvent was removed by rotary evaporation under reduced pressure
  6. washthe resulting residue was subjected to flash column chromatography (silica gel; gradient elution EtOAc/hexane 2/9815/85)
  7. customRemoval of excess eluent

출처 및 근거

ORD 기록
ord-0cb0669eb654438d8a7c3c8d43450557
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08940733B2

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