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2-Methyl-3-butyn-2-ol → 9-(3-Hydroxy-3-methylbut-1-yn-1-yl)-3-methyl-3,4,5,6-tetrahydro-4,6-methanobenzo[3,4]cyclohept a[1,2-d]imidazole-2-carboxamide

HRID 575445
ノート
印刷プレビュー

反応式

HRID 575445 の反応式
I[C:2]1[CH:3]=[CH:4][C:5]2[CH:18]3[CH2:19][CH:16]([CH2:17]3)[C:8]3[N:9]([CH3:15])[C:10]([C:12]([NH2:14])=[O:13])=[N:11][C:7]=3[C:6]=2[CH:20]=1.[CH3:21][C:22]([OH:26])([C:24]#[CH:25])[CH3:23]>N1CCCCC1.[Cu]I.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>[OH:26][C:22]([CH3:23])([CH3:21])[C:24]#[C:25][C:2]1[CH:3]=[CH:4][C:5]2[CH:18]3[CH2:19][CH:16]([CH2:17]3)[C:8]3[N:9]([CH3:15])[C:10]([C:12]([NH2:14])=[O:13])=[N:11][C:7]=3[C:6]=2[CH:20]=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 2

HCID 82582-Methyl-3-butyn-2-olHCID 866935079-Iodo-3-methyl-3,4,5,6-tetrahydro-4,6-methanobenzo[3,4]cyclohepta[1,2-d]imidazole-2-carboxamide

生成物 1

HCID 866935069-(3-Hydroxy-3-methylbut-1-yn-1-yl)-3-methyl-3,4,5,6-tetrahydro-4,6-methanobenzo[3,4]cyclohept a[1,2-d]imidazole-2-carboxamide収率 4.2%

試薬・触媒・溶媒 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)触媒
HCID 178418397
HCID 178418397、化合物
触媒
HCID 8082Piperidine溶媒

反応条件

温度
40 °C

実験手順

To a solution 9-iodo-3-methyl-3,4,5,6-tetrahydro-4,6-methanobenzo[3,4]cyclohepta[1,2-d]imidazole-2-carboxamide (100 mg, 0.26 mmol) in piperidine (2 mL) was introduced 2-methyl-3-butyn-2-ol (89 mg, 1.05 mmol) and copper(I) iodide (2.5 mg, 0.01 mmol). The solution was de-oxygenated by nitrogen bubbling for five minutes, then tetrakis(triphenylphosphine)palladium(0) (15 mg, 0.01 mmol) added and bubbling continued for a further two minutes. The pressure tube was closed under an atmosphere of nitrogen and the reaction mixture warmed to 40° C. for 2.5 hr. After evaporation of the reaction mixture in vacuo, the residue was suspended in ethyl acetate (25 mL) and washed with saturated aqueous sodium bicarbonate (6 mL), water (2×10 mL) and brine (5 mL). The organic extract was dried over sodium sulfate, filtered, and the filtrate adsorbed onto silica gel in vacuo. Purification of the dry-loaded material by silica gel flash column chromatography (eluent: heptane/ethyl acetate gradient) was followed by suspension of the product in acetonitrile (0.6 mL). The solid was collected by filtration to furnish the title compound (4.5 mg, 0.011 mmol, 4%) as a colorless solid: 1H NMR (500 MHz, CDCl3) delta 1.65 (s, 6H), 1.71 (d, J=9.46 Hz, 2H), 2.15 (br. s., 1H), 2.91-3.00 (m, 2H), 3.48 (td, J=7.41, 3.78 Hz, 1H), 3.65 (td, J=8.04, 3.47 Hz, 1H), 4.01 (s, 3H), 5.37 (br. s., 1H), 7.03 (d, J=7.57 Hz, 1H), 7.14 (dd, J=7.72, 1.42 Hz, 1H), 7.49 (br. s., 1H), 8.47 (br. s., 1H); LC-MS: m/z=+336.10 (M+H)+

後処理

  1. custombubbling
  2. waitcontinued for a further two minutes
  3. customThe pressure tube was closed under an atmosphere of nitrogen
  4. customAfter evaporation of the reaction mixture in vacuo
  5. washwashed with saturated aqueous sodium bicarbonate (6 mL), water (2×10 mL) and brine (5 mL)
  6. extractionThe organic extract
  7. dry with materialwas dried over sodium sulfate
  8. filtrationfiltered
  9. customPurification of the dry-loaded material by silica gel flash column chromatography (eluent: heptane/ethyl acetate gradient)
  10. additionwas followed by suspension of the product in acetonitrile (0.6 mL)
  11. filtrationThe solid was collected by filtration

出典と根拠

ORDレコード
ord-cbfbc9c3aa954b478426ba8600f5caf0
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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