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Ethyl Acetate → Tert-butyl 3-[(5-bromo-4-methyl-2H-indazol-2-yl)methyl]-azetidin-1-carboxylate

HRID 2174927
ノート
印刷プレビュー

反応式

HRID 2174927 の反応式
[Br:1][C:2]1[C:3]([CH3:11])=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][N:6]=[CH:5]2.[C:12]([O:16][C:17]([N:19]1[CH2:22][CH:21]([CH2:23]OS(C2C=CC(C)=CC=2)(=O)=O)[CH2:20]1)=[O:18])([CH3:15])([CH3:14])[CH3:13].C[Si]([N-][Si](C)(C)C)(C)C.[Na+].C(OCC)(=O)C>O1CCOCC1.O1CCCC1.O>[Br:1][C:2]1[CH:10]=[CH:9][C:8]2[C:4](=[CH:5][N:6]([CH2:23][CH:21]3[CH2:22][N:19]([C:17]([O:16][C:12]([CH3:13])([CH3:15])[CH3:14])=[O:18])[CH2:20]3)[N:7]=2)[C:3]=1[CH3:11]
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

8

反応物 4

HCID 8857Ethyl AcetateHCID 2724254Sodium bis(trimethylsilyl)amideHCID 441192325-Bromo-4-methyl-1H-indazoleHCID 56777214Tert-butyl 3-(tosyloxymethyl)azetidine-1-carboxylate

生成物 1

HCID 117690535Tert-butyl 3-[(5-bromo-4-methyl-2H-indazol-2-yl)methyl]-azetidin-1-carboxylate

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 8028Tetrahydrofuran溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
90 °C

実験手順

To a solution of 21.1 g of 5-bromo-4-methyl-1H-indazole and 37.6 g of tert-butyl-3-[(tosyloxy)-methyl]azetidin-1-carboxylate in 100 ml dioxan were added 150 ml of a 1M solution of sodium bis(trimethylsilyl)amide in tetrahydrofuran at 25° C. and this was stirred for 6 hrs at 90° C. After cooling, the reaction mixture was treated with ethyl acetate and water, the organic phases separated and the aqueous phase extracted twice with 100 ml portions of ethyl acetate. The combined organic phases were washed with saturated sodium chloride solution, dried over sodium sulphate, and concentrated in vacuo after filtration.

後処理

  1. temperatureAfter cooling
  2. customthe organic phases separated
  3. extractionthe aqueous phase extracted twice with 100 ml portions of ethyl acetate
  4. washThe combined organic phases were washed with saturated sodium chloride solution
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated in vacuo
  7. filtrationafter filtration

出典と根拠

ORDレコード
ord-20781fbff8cc45bc8a8d2d772b8723e5
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09062041B2

反応ノート

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