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Water → HCID 86655219、化合物

HRID 1256133
ノート
印刷プレビュー

反応式

HRID 1256133 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([S:12](=[O:25])(=[O:24])[NH:13][C:14]2[CH:15]=[CH:16][C:17]3[CH2:21][O:20][B:19]([OH:22])[C:18]=3[CH:23]=2)=[C:6]([CH2:8][C:9]([OH:11])=O)[CH:7]=1.Cl.[CH3:27][O:28][NH2:29].C1CN([P+](ON2N=NC3C=CC=CC2=3)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F.O>CN(C=O)C>[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([S:12](=[O:25])(=[O:24])[NH:13][C:14]2[CH:15]=[CH:16][C:17]3[CH2:21][O:20][B:19]([OH:22])[C:18]=3[CH:23]=2)=[C:6]([CH2:8][C:9]([NH:29][O:28][CH3:27])=[O:11])[CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 521874O-Methylhydroxylamine hydrochlorideHCID 2724699PyBOPHCID 53234452HCID 53234452、化合物

生成物 1

HCID 86655219HCID 86655219、化合物収率 4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a stirred solution of 2-(5-amino-2-(N-(1-hydroxy-1,3-dihydrobenzo[c][1,2]oxaborol-6-yl)sulfamoyl)phenyl)acetic acid (430 mg, 1.19 mmol) and methoxyamine hydrochloride (125 mg, 1.78 mmol) in 10 mL of DMF was added PyBOP (926 mg, 1.78 mmol) and TEA (496 uL, 3.56 mmol). The reaction mixture was stirred for 16 hours. After water was added, the reaction mixture was extracted with ethyl acetate and washed with water, 1N HCl and brine. The organic layer was dried over Na2SO4 and concentrated. The crude residue was purified by prep HPLC (SunFire Prep C18 OBD 5 uM 30×50 mm column) to give the desired product as a yellow solid (16.4 mg, yield 4%). Analytical data for title compound. MS calcd for (C16H18BN3O6S): 391.2. MS found (ESI negative): (M−H)−=390.0. 1H NMR (DMSO-d6) δ (ppm): 11.14 (s, 1H), 9.74 (s, 1H), 9.10 (bs, 1H), 7.36-7.40 (m, 2H), 7.16 (d, J=8.0 Hz, 1H), 7.05 (d, J=8.0 Hz, 1H), 6.36 (s, 1H), 6.31 (d, J=8.8 Hz, 1H), 4.80 (s, 2H), 3.58 (s, 2H), 3.56 (s, 3H).

後処理

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washwashed with water, 1N HCl and brine
  3. dry with materialThe organic layer was dried over Na2SO4
  4. concentrationconcentrated
  5. customThe crude residue was purified by prep HPLC (SunFire Prep C18 OBD 5 uM 30×50 mm column)

出典と根拠

ORDレコード
ord-d07b3d5efea548c1ab759b7f88dcf2a5
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08461134B2

反応ノート

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