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Diisopropylethylamine → cis 3-(1-benzenesulfonyl-5-nitro-1H-pyrrolo[2,3-b]pyridine-4-ylamino)cyclohexanecarbonitrile

HRID 1257718
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HRID 1257718 반응식
[C:1]1([S:7]([N:10]2[C:14]3=[N:15][CH:16]=[C:17]([N+:20]([O-:22])=[O:21])[C:18](Cl)=[C:13]3[CH:12]=[CH:11]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH2:23][CH:24]1[CH2:29][CH2:28][CH2:27][CH:26]([C:30]#[N:31])[CH2:25]1.C(N(C(C)C)CC)(C)C>CC(O)C>[C:1]1([S:7]([N:10]2[C:14]3=[N:15][CH:16]=[C:17]([N+:20]([O-:22])=[O:21])[C:18]([NH:23][C@@H:24]4[CH2:29][CH2:28][CH2:27][C@H:26]([C:30]#[N:31])[CH2:25]4)=[C:13]3[CH:12]=[CH:11]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
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참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 215121773-AminocyclohexanecarbonitrileHCID 583947741-(benzenesulfonyl)-4-chloro-5-nitro-1H-pyrrolo(2,3-b)pyridine

생성물 1

HCID 86656736cis 3-(1-benzenesulfonyl-5-nitro-1H-pyrrolo[2,3-b]pyridine-4-ylamino)cyclohexanecarbonitrile수율 23.5%

시약·촉매·용매 1

HCID 3776Isopropanol
용매

실험 절차

A mixture of 1-benzenesulfonyl-4-chloro-5-nitro-1H-pyrrolo[2,3-b]pyridine (1.01 g, 3.00 mmol), 3-amino-cyclohexanecarbonitrile (3.30 mmol assumed) and diisopropylethylamine (2.60 mL, 15.0 mmol) in propan-2-ol (30 mL) were heated to reflux for 2 hours. The cooled reaction mixture was filtered and the yellow solid further purified by column chromatography on silica gel (gradient: 0 to 10% ethyl acetate in toluene) to afford 300 mg (23%) of cis 3-(1-benzenesulfonyl-5-nitro-1H-pyrrolo[2,3-b]pyridine-4-ylamino)cyclohexanecarbonitrile. 1H NMR (400 MHz, DMSO) δ: 8.90 (s, 1H), 8.80 (d, 1H), 8.13 (m, 2H), 7.84 (d, 1H), 7.76 (m, 1H), 7.66 (m 2H), 7.09 (d, 1H), 4.11 (m, 1H), 3.10 (m, 1H), 2.28 (m, 1H), 1.98 (m, 2H), 1.79 (m, 2H), 1.50 (m, 3H). The filtrate was concentrated and purified by column chromatography on silica gel (gradient: 0 to 10% ethyl acetate in toluene) to afford 220 mg (17%) of trans 3-(1-benzenesulfonyl-5-nitro-1H-pyrrolo[2,3-b]pyridine-4-ylamino)cyclohexanecarbonitrile. LCMS (Method I, ESI): RT=3.76 min, m+H=426.1; 1H NMR (400 MHz, DMSO) δ: 8.92 (s, 1H), 8.13 (dd, 2H), 7.88 (d, 1H), 7.77 (t, 1H), 7.65 (t, 2H), 6.99 (d, 1H), 4.27 (m, 1H), 3.26 (m, 1H), 2.18 (m, 1H), 1.99 (m, 1H), 1.91 (m, 1H), 1.83-1.58 (m, 5H).

후처리

  1. temperaturewere heated
  2. temperatureto reflux for 2 hours
  3. customThe cooled reaction mixture
  4. filtrationwas filtered
  5. customthe yellow solid further purified by column chromatography on silica gel (gradient: 0 to 10% ethyl acetate in toluene)

출처 및 근거

ORD 기록
ord-1d183f507fa14aad9d14c1b8952cc507
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08461328B2

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