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Sodium Iodide → HCID 86693510、化合物

HRID 575448
ノート
印刷プレビュー

反応式

HRID 575448 の反応式
[I:1][C:2]1[CH:3]=[CH:4][C:5]2[CH:19]3[CH2:20][CH:17]([CH2:18]3)[C:8]3[NH:9][C:10]([C:12]([O:14][CH2:15][CH3:16])=[O:13])=[N:11][C:7]=3[C:6]=2[CH:21]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+].Cl[CH2:31][C:32]1[C:40]2[C:35](=[CH:36][CH:37]=[CH:38][CH:39]=2)[N:34]([CH3:41])[N:33]=1>CN(C)C=O>[I:1][C:2]1[CH:3]=[CH:4][C:5]2[CH:19]3[CH2:18][CH:17]([CH2:20]3)[C:8]3[N:9]([CH2:31][C:32]4[C:40]5[C:35](=[CH:36][CH:37]=[CH:38][CH:39]=5)[N:34]([CH3:41])[N:33]=4)[C:10]([C:12]([O:14][CH2:15][CH3:16])=[O:13])=[N:11][C:7]=3[C:6]=2[CH:21]=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

6

反応物 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 75374703-(chloromethyl)-1-methyl-1H-indazoleHCID 86693505HCID 86693505、化合物

生成物 1

HCID 86693510HCID 86693510、化合物収率 97.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

反応条件

温度
50 °C

実験手順

To a mixture of ethyl 9-iodo-3,4,5,6-tetrahydro-4,6-methanobenzo[3,4]cyclohepta[1,2-d]imidazole-2-carboxylate (150 mg, 0.38 mmol), potassium carbonate (79 mg, 0.57 mmol) and sodium iodide (114 mg, 0.76 mmol) was introduced a solution of 3-(chloromethyl)-1-methyl-1H-indazole (137 mg, 0.76 mmol) in N,N-dimethylformamide (5 mL). After warming to 50° C. for 2 hr the reaction mixture was evaporated in vacuo. The residue was suspended in ethyl acetate (40 mL), washed with saturated aqueous sodium bicarbonate (15 mL). After washing the basic aqueous extract with ethyl acetate (3×10 ml), all the organic extracts were combined, washed with water (15 mL) and brine (15 mL), and dried over sodium sulfate. Following filtration of the ethyl acetate extract, the filtrate was evaporated onto silica gel in vacuo. The dry-loaded material was purified by silica gel flash column chromatography (eluent: heptanes/ethyl acetate gradient) to furnish the title compound (198 mg, 0.37 mmol, 97%) as a colorless solid: 1H NMR (500 MHz, CDCl3) δ1.48 (t, J=7.2 Hz, 3H), 1.55-1.57 (m, 2H), 2.79 (dq, J=8.2, 2.8 Hz, 2H), 3.53 (td, J=7.9, 3.8 Hz, 1H), 3.73 (td, J=7.6, 4.1 Hz, 1H), 3.99 (s, 3H), 4.50 (q, J=7.2 Hz, 2H), 6.13 (s, 2H), 6.77 (d, J=7.8 Hz, 1H), 7.05 (ddd, J=7.9, 6.3, 1.3 Hz, 1H), 7.32-7.34 (m, 3H), 7.41 (dd, J=7.9, 1.9 Hz, 1H), 8.89 (s, 1H); M+H=539.

後処理

  1. customwas evaporated in vacuo
  2. washwashed with saturated aqueous sodium bicarbonate (15 mL)
  3. washAfter washing the basic
  4. extractionaqueous extract with ethyl acetate (3×10 ml), all the organic extracts
  5. washwashed with water (15 mL) and brine (15 mL)
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltration of the ethyl acetate
  8. extractionextract
  9. customthe filtrate was evaporated onto silica gel in vacuo
  10. customThe dry-loaded material was purified by silica gel flash column chromatography (eluent: heptanes/ethyl acetate gradient)

出典と根拠

ORDレコード
ord-56c44b7742bd49b88dfcda25551f1bde
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09034866B2

反応ノート

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