Methyl iodide → HCID 57679159、化合物

HRID 492150ノート

反応式

HRID 492150 の反応式
[C:1]([O:5][C:6](=[O:24])[NH:7][CH2:8][C:9]1([CH2:18][CH:19]2[O:23][CH2:22][CH2:21][O:20]2)[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11][CH2:10]1)([CH3:4])([CH3:3])[CH3:2].IC.[CH3:27][Si]([N-][Si](C)(C)C)(C)C.[Na+]>C1COCC1>[C:1]([O:5][C:6](=[O:24])[N:7]([CH2:8][C:9]1([CH2:18][CH:19]2[O:23][CH2:22][CH2:21][O:20]2)[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11][CH2:10]1)[CH3:27])([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 2724254Sodium bis(trimethylsilyl)amideHCID 57679134tert-butyl [1-(1,3-dioxolan-2-ylmethyl)-2,3-dihydro-1H-inden-1-yl]methylcarbamate

生成物 1

HCID 57679159HCID 57679159、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of tert-butyl[1-(1,3-dioxolan-2-ylmethyl)-2,3-dihydro-1H-inden-1-yl]methylcarbamate (13.50 g, 38.9 mmole) in THF was cooled to 0° C. To this was added iodomethane (7.27 ml, 117 mmole) followed by 1M NaHMDS in THF (58 ml, 58 mmole). The reaction was then warmed to room temperature and stirred until no U16370/185/2 remained by TLC. The THF was evaporated and the residue dissolved in Et2O. The ether was washed with water and evaporated to afford 14.33 g of tert-butyl[1-(1,3-dioxolan-2-ylmethyl)-2,3-dihydro-1H-inden-1-yl]methyl(methyl)carbamate as a crude oil, which was used, with no further purification.

後処理

  1. customThe THF was evaporated
  2. dissolutionthe residue dissolved in Et2O
  3. washThe ether was washed with water
  4. customevaporated

出典と根拠

ORDレコード
ord-8b74e1d4819b4bf0975073885031e435
出典データセット
uspto-grants-2009_05
特許番号
US07531661B2

反応ノート

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