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Sodium Hydroxide → HCID 59596464、化合物

HRID 2264960
ノート
印刷プレビュー

反応式

HRID 2264960 の反応式
C(O[C:4]([C:6]1[N:14]([CH3:15])[C:13]2[CH:12]=[CH:11][N:10]=[C:9](CC)[C:8]=2[C:7]=1[NH:18][C:19]1[CH:24]=[CH:23][C:22]([I:25])=[CH:21][C:20]=1[F:26])=[O:5])C.[OH-].[Na+].[CH:29]([O:31][CH2:32][CH2:33][O:34][NH2:35])=[CH2:30].CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.CCN(C(C)C)C(C)C>C1COCC1.CO>[CH:29]([O:31][CH2:32][CH2:33][O:34][NH:35][C:4]([C:6]1[N:14]([CH3:15])[C:13]2[CH:12]=[CH:11][N:10]=[CH:9][C:8]=2[C:7]=1[NH:18][C:19]1[CH:24]=[CH:23][C:22]([I:25])=[CH:21][C:20]=1[F:26])=[O:5])=[CH2:30]
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

9

反応物 6

HCID 14798Sodium HydroxideHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 21867017O-(2-(Vinyloxy)ethyl)hydroxylamineHCID 67212327HCID 67212327、化合物

生成物 1

HCID 59596464
HCID 59596464、化合物
収率 57%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
65 °C

実験手順

A mixture of ethyl 3-(2-fluoro-4-iodo-phenylamino)-1-methyl-1H-pyrrolo[3,2-c]pyridine-2-carboxylic acid ethyl ester (100 mg, 0.23 mmol), 1N aqueous sodium hydroxide (0.25 ml) and MeOH (3.0 ml) was heated at 65° C. for 1.5 hours. The reaction mixture was concentrated and azeotroped with toluene (2×2 ml) to give a solid residue. The solid residue was dissolved in anhydrous THF (4 ml) and O-(2-vinyloxy-ethyl)-hydroxylamine (47 mg, 0.46 mmol), EDCI (55 mg, 0.29 mmol), HOBt (43 mg, 0.32 mmol) and DIPEA (119 μl, 0.68 mmol) were added. After stirring for 72 hours at ambient temperature, the mixture was evaporated and the residue was partitioned between ethyl acetate (30 ml) and water (20 ml). The organic layer was isolated, dried over sodium sulphate, then filtered and evaporated to give a yellow oil. The oil was purified by flash chromatography (Si-PPC, dichloromethane:methanol, gradient 100:0 to 90:10) to afford the title compound as a yellow solid (64 mg, 57%). LCMS (method B): RT=2.20 min, M+H+=497.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. customazeotroped with toluene (2×2 ml)
  3. customto give a solid residue
  4. customthe mixture was evaporated
  5. customthe residue was partitioned between ethyl acetate (30 ml) and water (20 ml)
  6. customThe organic layer was isolated
  7. dry with materialdried over sodium sulphate
  8. filtrationfiltered
  9. customevaporated
  10. customto give a yellow oil
  11. customThe oil was purified by flash chromatography (Si-PPC, dichloromethane:methanol, gradient 100:0 to 90:10)

出典と根拠

ORDレコード
ord-7c0f11d6811049da82a97cc7130e6484
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07855216B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート