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Sodium Carbonate → HCID 145857603, 화합물

HRID 2216165
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HRID 2216165 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH3:9])=[CH:4][C:3]=1[CH3:10].C1(P(C2CCCCC2)C2C=CC=CC=2C2C=CC=CC=2)CCCCC1.B([O-])[O-].[C:39]([O:43][C:44](=[O:65])[NH:45][C:46]([C:48]1[S:49][C:50]([S:63][CH3:64])=[C:51]([S:53]([C:56]2[CH:61]=[CH:60][CH:59]=[C:58](Br)[CH:57]=2)(=[O:55])=[O:54])[CH:52]=1)=[NH:47])([CH3:42])([CH3:41])[CH3:40].C([O-])([O-])=O.[Na+].[Na+]>O1CCOCC1.C(O)C.C1(C)C=CC=CC=1.C([O-])(=O)C.[Pd+2].C([O-])(=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>[C:39]([O:43][C:44](=[O:65])[NH:45][C:46](=[NH:47])[C:48]1[S:49][C:50]([S:63][CH3:64])=[C:51]([S:53]([C:56]2[CH:61]=[C:60]([C:2]3[CH:7]=[CH:6][C:5]([NH:8][CH3:9])=[CH:4][C:3]=3[CH3:10])[CH:59]=[CH:58][CH:57]=2)(=[O:55])=[O:54])[CH:52]=1)([CH3:42])([CH3:40])[CH3:41]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 5

HCID 10340Sodium CarbonateHCID 27342162-(Dicyclohexylphosphino)biphenylHCID 218865734-Bromo-n,3-dimethylanilineHCID 145857672tert-butyl N-[4-(3-bromophenyl)sulfonyl-5-methylsulfanylthiophene-2-carboximidoyl]carbamateHCID 178514824HCID 178514824, 화합물

생성물 1

HCID 145857603
HCID 145857603, 화합물
수율 62%

시약·촉매·용매 5

HCID 167845palladium(II) acetate촉매HCID 178418397HCID 178418397, 화합물촉매HCID 702Ethanol용매HCID 1140Toluene용매HCID 312751,4-Dioxane용매

실험 절차

The procedure in Example 294: step e was followed using (4-bromo-3-methyl-phenyl)-methyl-amine ((Example 262: step a) 600 mg, 3 mmol), palladium acetate (34 mg, 0.15 mmol), and 2-(dicyclohexylphosphino)biphenyl (210 mg, 0.6 mmol) in dioxane (20 mL). Analogous workup yielded the crude pinacolboronate ester (720 mg, 98%) which was used without further purification. Following the procedure in Example 294: step f the crude boronate (540 mg, 2.18 mmol) was reacted with {[4-(3-bromo-benzenesulfonyl)-5-methylsulfanyl-thiophen-2-yl]-imino-methyl}-carbamic acid tert-butyl ester ((Example 27: step c) 715 mg, 1.46 mmol), aq Na2CO3 (2M, 4.4 mL, 8.8 mL), and Pd(PPh3)4 (407 mg, 0.37 mmol) in ethanol (4.4 mL) and toluene (8.8 mL). Analogous workup and SiO2 flash column chromatography yielded the title compound (482 mg, 62%) as a yellow glass. 1H-NMR (CDCl3): δ 8.0 (s, 1H), 7.95 (m, 1H), 7.90 (m, 1H), 7.55 (m, 1H), 7.51 (m, 1H), 7.05 (m, 1H), 6.53 (m, 2H), 2.9 (s, 3H), 2.56 (s, 3H), 2.56 (s, 3H), 2.22 (s, 3H), 1.52 (s, 9H).

후처리

  1. customAnalogous workup yielded the crude pinacolboronate ester (720 mg, 98%) which
  2. customwas used without further purification

출처 및 근거

ORD 기록
ord-04901857444a45e2930c640c94d8eef4
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07109354B2

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