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Sodium Carbonate → HCID 24985251、化合物

HRID 1724062
ノート
印刷プレビュー

反応式

HRID 1724062 の反応式
I[C:2]1[CH:19]=[CH:18][C:5]([CH2:6][N:7]2[CH2:11][C:10]3([CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]3)[O:9][C:8]2=[O:17])=[CH:4][CH:3]=1.[CH2:20]([N:27]1[CH2:32][CH2:31][O:30][CH:29](B(O)O)[CH2:28]1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(=O)([O-])[O-].[Na+].[Na+]>COCCOC.ClCCl.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[N:27]1([CH2:20][C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:26]=2[C:2]2[CH:19]=[CH:18][C:5]([CH2:6][N:7]3[CH2:11][C:10]4([CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]4)[O:9][C:8]3=[O:17])=[CH:4][CH:3]=2)[CH2:28][CH2:29][O:30][CH2:31][CH2:32]1
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 3

HCID 10340Sodium CarbonateHCID 57559818HCID 57559818、化合物HCID 68546700HCID 68546700、化合物

生成物 1

HCID 24985251HCID 24985251、化合物収率 83.5%

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒HCID 6344
Dichloromethane
溶媒
HCID 80711,2-Dimethoxyethane溶媒

実験手順

3-(4-Iodo-benzyl)-1-oxa-3-aza-spiro[4.5]decan-2-one (55 mg, 0.148 mmol) and benzylmopholine-2-boronic acid (49 mg, 0.222 mmol) were mixed in ethylene glycol dimethyl ether (1 mL) and sodium carbonate (2M) aqueous solution (1 mL). Tetrakis(triphenylphosphine)palladium (Pd(PPh3)4) (17 mg, 0.0148 mmol) was added and the reaction mixture was heated at 100˜110° C. for 1˜1.5 hours. The reaction was diluted with dichloromethane (DCM), washed with water (4 mL) and brine (4 mL). The organic phase was separated, dried over anhydrous sodium sulfate and concentrated. The crude residue was purified on silica gel eluting with 5-30% ethyl acetate in hexane to give the product as off-white solid (52 mg, 83%). 1H NMR (300 MHz, CDCl3): δ 7.49 (m, 1H), 7.42 (d, 2H), 7.32 (m, 5H), 4.5 (s, 2H), 3.65 (t, 4H), 3.39 (s, 2H), 3.18 (s, 2H), 2.36 (t, 4H), 1.82 (m, 4H), 1.54 (m, 6H).

後処理

  1. temperaturethe reaction mixture was heated at 100˜110° C. for 1˜1.5 hours
  2. washwashed with water (4 mL) and brine (4 mL)
  3. customThe organic phase was separated
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customThe crude residue was purified on silica gel eluting with 5-30% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-175fe6edd2cc4854944d4916159c38a3
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07485722B2

反応ノート

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