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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 86656241、化合物

HRID 79048
ノート
印刷プレビュー

反応式

HRID 79048 の反応式
[F:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[C:18]([C:19]([OH:21])=O)=[CH:17][CH:16]=[C:15]2[C:11]=1[CH:12]=[N:13][N:14]2[S:22]([C:25]1[CH:30]=[CH:29][C:28]([CH3:31])=[CH:27][CH:26]=1)(=[O:24])=[O:23].CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.[CH:53]([O:55][CH2:56][CH2:57][O:58][NH2:59])=[CH2:54].CCN(C(C)C)C(C)C>CN(C=O)C>[CH:53]([O:55][CH2:56][CH2:57][O:58][NH:59][C:19]([C:18]1[C:10]([NH:9][C:3]2[CH:4]=[CH:5][C:6]([I:8])=[CH:7][C:2]=2[F:1])=[C:11]2[C:15](=[CH:16][CH:17]=1)[N:14]([S:22]([C:25]1[CH:30]=[CH:29][C:28]([CH3:31])=[CH:27][CH:26]=1)(=[O:23])=[O:24])[N:13]=[CH:12]2)=[O:21])=[CH2:54]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 21867017O-(2-(Vinyloxy)ethyl)hydroxylamineHCID 670840434-(2-Fluoro-4-iodo-phenylamino)-1-(toluene-4-sulfonyl)-1H-indazole-5-carboxylic acid

生成物 1

HCID 86656241
HCID 86656241、化合物
収率 66%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 4-(2-fluoro-4-iodo-phenylamino)-1-(toluene-4-sulfonyl)-1H-indazole-5-carboxylic acid (0.58 g, 1.05 mmol) in DMF (10 mL) was added EDCI (0.22 g, 1.1 mmol) followed by HOBt (0.16 g, 1.1 mmol) and the reaction mixture stirred at room temperature for 10 minutes. O-(2-vinyloxy-ethyl)-hydroxylamine (0.12 g, 1.1 mmol) and DIPEA (0.2 mL, 1.1 mmol) were added and the reaction stirred for 16 hours before being concentrated in vacuo. The resultant residue was dissolved in ethyl acetate (10 mL), washed with an aqueous saturated sodium bicarbonate solution (10 mL) before the aqueous fraction was extracted twice with ethyl acetate (2×10 mL). The combined organic extracts were washed with brine (20 mL), dried (MgSO4) and concentrated in vacuo. The resultant residue was subjected to flash chromatography (Si—PPC, gradient 0-100% ethyl acetate in cyclohexane) to yield the title compound as a pale brown solid (439 mg, 66%). LCMS (Method B): RT=4.40 min, [M+H]+=637.

後処理

  1. stirringthe reaction stirred for 16 hours
  2. concentrationbefore being concentrated in vacuo
  3. dissolutionThe resultant residue was dissolved in ethyl acetate (10 mL)
  4. washwashed with an aqueous saturated sodium bicarbonate solution (10 mL) before the aqueous fraction
  5. extractionwas extracted twice with ethyl acetate (2×10 mL)
  6. washThe combined organic extracts were washed with brine (20 mL)
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-4bab65d3e5eb4a26ab6cd9f33c425431
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08841462B2

反応ノート

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