Methyl iodide → HCID 57679159, 화합물

HRID 492150노트

반응식

HRID 492150 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 57679159HCID 57679159, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-8b74e1d4819b4bf0975073885031e435
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07531661B2

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