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Ozone → 4-[2-(4-tert-Butyl-phenyl)-3H-imidazo[4,5-c]pyridin-7-yl]-piperazine-1-carboxylic acid benzyl ester

HRID 729355
ノート
印刷プレビュー

反応式

HRID 729355 の反応式
[CH2:1]([O:8][C:9]([N:11]1[CH2:15][CH:14]=[CH:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O=[O+][O-].P(OCC)(OCC)OCC.[C:29]([C:33]1[CH:38]=[CH:37][C:36]([C:39]2[NH:40][C:41]3[C:46]([NH2:47])=[CH:45][N:44]=[CH:43][C:42]=3[N:48]=2)=[CH:35][CH:34]=1)([CH3:32])([CH3:31])[CH3:30].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>C(Cl)Cl.CO>[CH2:1]([O:8][C:9]([N:11]1[CH2:15][CH2:14][N:47]([C:46]2[C:41]3[N:40]=[C:39]([C:36]4[CH:37]=[CH:38][C:33]([C:29]([CH3:32])([CH3:31])[CH3:30])=[CH:34][CH:35]=4)[NH:48][C:42]=3[CH:43]=[N:44][CH:45]=2)[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 24823OzoneHCID 31215Triethyl phosphiteHCID 643471Benzyl 3-pyrroline-1-carboxylateHCID 5049666Sodium triacetoxyborohydrideHCID 178440764HCID 178440764、化合物

生成物 1

HCID 578327604-[2-(4-tert-Butyl-phenyl)-3H-imidazo[4,5-c]pyridin-7-yl]-piperazine-1-carboxylic acid benzyl ester
収率 2.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
-78 °C

実験手順

2,5-Dihydro-pyrrole-1-carboxylic acid benzyl ester 6 was dissolved in DCM (5 ml) and MeOH (2 ml). It was cooled to −78° C. and treated with ozone until it was blue in color. Triethyl phosphite (246 mg, 1.48 mmol) was added and the solution was allowed to stir for 5 minutes. 2-(4-tert-Butyl-phenyl)-1H-imidazo[4,5-c] pyridin-7-ylamine 4 (266 mg, 1.00 mmol) was added followed by sodium triacetoxyborohydride (538 mg, 2.54 mmol). This mixture was allowed to stir for 18 hours. Mass spectroscopy showed no starting material left after this time, and the solvent was removed under vacuum. The crude was taken up in ethyl acetate and washed with a saturated sodium bicarbonate solution, brine, dried over MgSO4, and the crude was purified by HPLC (Method E), yielding the title product 7 (12 mg (2.5%), 0.026 mmol). 1H NMR (DMSO-d6): δ 8.88 (bs, 1H), 8.23 (d, J=8.5 Hz, 2H), 7.96 (s, 1H), 7.68 (d, J=8.5 Hz, 2H), 7.38 (m, 5H), 5.15 (s, 2H), 1.33 (s, 9H). MS (ESI-POS): [M+H]+=470; MS(ESI-NEG):[M−H]−=468.

後処理

  1. stirringto stir for 18 hours
  2. waitleft after this time
  3. customthe solvent was removed under vacuum
  4. washwashed with a saturated sodium bicarbonate solution, brine
  5. dry with materialdried over MgSO4
  6. customthe crude was purified by HPLC (Method E)

出典と根拠

ORDレコード
ord-ad390ac47f0c4b5e9dc6f68d48e90946
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07582634B2

反応ノート

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