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Methyl iodide → tert-butyl N-(2-chloro-3-methylfuro[2,3-c]pyridin-7-yl)-N-[(2-methylpropan-2-yl)oxycarbonyl]carbamate

HRID 389425
ノート
印刷プレビュー

反応式

HRID 389425 の反応式
[Cl:1][C:2]1[O:25][C:5]2=[C:6]([N:10]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[N:7]=[CH:8][CH:9]=[C:4]2[CH:3]=1.[Li+].[CH3:27]C([N-]C(C)C)C.CI>C1COCC1>[Cl:1][C:2]1[O:25][C:5]2=[C:6]([N:10]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[N:7]=[CH:8][CH:9]=[C:4]2[C:3]=1[CH3:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 2724682Lithium diisopropylamideHCID 66760259HCID 66760259、化合物

生成物 1

HCID 66760298tert-butyl N-(2-chloro-3-methylfuro[2,3-c]pyridin-7-yl)-N-[(2-methylpropan-2-yl)oxycarbonyl]carbamate収率 102.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Di-tert-butyl (2-chlorofuro[2,3-c]pyridin-7-yl)imidodicarbonate (3.0 g, 8.15 mmol) in dry THF (100 mL) was cooled to −65° C. to −75° C. and LDA (1.8 M in THF/heptanes/ethylbenzene, 6.0 mL, 10.8 mmol), pre-cooled to the same temperature, was added slowly via syringe over a period of 10 min. The mixture was stirred for 1.5 h at −65° C. to −75° C. and then treated with methyl iodide (0.76 mL, 12.2 mmol) in dry THF added slowly via syringe. The mixture was allowed to warm to RT overnight and was quenched by the addition of water (50 mL) and diluted with EtOAc (100 mL). The phases were separated and the organic phase was dried over Na2SO4, and concentrated in vacuo leaving 3.2 g of a brown solid which was used without further purification. 1H NMR (400 MHz, CDCl3): δ 8.25 (d, J=5.5 Hz, 1H), 7.39 (d, J=5.5 Hz, 1H), 2.22 (s, 3H), 1.40 (s, 18H).

後処理

  1. additionwas added slowly via syringe over a period of 10 min
  2. additionadded slowly via syringe
  3. customwas quenched by the addition of water (50 mL)
  4. additiondiluted with EtOAc (100 mL)
  5. customThe phases were separated
  6. dry with materialthe organic phase was dried over Na2SO4
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-9ae425002bf5418b8fbf69cb235c7c18
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08378104B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート