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Sodium Azide → (S)-2'-azido-7'-methoxy-5H-spiro[oxazole-4,9'-xanthen]-2-amine

HRID 1970308
ノート
印刷プレビュー

反応式

HRID 1970308 の反応式
Br[C:2]1[CH:15]=[CH:14][C:13]2[O:12][C:11]3[C:6](=[CH:7][C:8]([O:16][CH3:17])=[CH:9][CH:10]=3)[C@:5]3([CH2:21][O:20][C:19]([NH2:22])=[N:18]3)[C:4]=2[CH:3]=1.[N-:23]=[N+:24]=[N-:25].[Na+].[Na].O=C1O[C@H]([C@H](CO)O)C(O)=C1O.CN[C@@H]1CCCC[C@H]1NC>CCO.O.[Cu]I>[N:23]([C:2]1[CH:15]=[CH:14][C:13]2[O:12][C:11]3[C:6](=[CH:7][C:8]([O:16][CH3:17])=[CH:9][CH:10]=3)[C@:5]3([CH2:21][O:20][C:19]([NH2:22])=[N:18]3)[C:4]=2[CH:3]=1)=[N+:24]=[N-:25]
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 33557Sodium AzideHCID 2733821trans-N,N'-dimethyl-1,2-cyclohexanediamineHCID 59272314(R)-2'-bromo-7'-methoxy-5H-spiro[oxazole-4,9'-xanthen]-2-amineHCID 66586226sodium L-ascorbic acid

生成物 1

HCID 86640718(S)-2'-azido-7'-methoxy-5H-spiro[oxazole-4,9'-xanthen]-2-amine

試薬・触媒・溶媒 3

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 702Ethanol溶媒
HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

A 5 mL smith synthesizer vial was charged with (R)-2′-bromo-7′-methoxy-5H-spiro[oxazole-4,9′-xanthen]-2-amine (1.248 g, 3.46 mmol), sodium azide (0.684 g, 10.52 mmol), L-ascorbic acid sodium salt (0.057 g, 0.288 mmol), copper(I) iodide (0.131 g, 0.688 mmol), and (1R,2R)—N1,N2-dimethylcyclohexane-1,2-diamine (0.116 mL, 0.736 mmol) in EtOH (6.0 mL), water (2.6 mL) and the reaction was heated to 100° C. in the microwave for 35 minutes. The reaction vial was cooled to RT and concentrated on the rotary evaporator and the resulting residue was taken up in ethyl acetate (125 mL), water (50 mL) the organic layer was separated. The organic layer was dried over sodium sulfate and concentrated to yield the crude product which was purified by silica gel flash column chromatography (using a 40G ISCO silica gel cartridge), and eluted using hexanes/ethyl acetate gradient. The fractions were combined and concentrated to yield (S)-2′-azido-7′-methoxy-5H-spiro[oxazole-4,9′-xanthen]-2-amine as a yellowish solid. MS (ESI pos. ion) m/z: 324 (M+1).

後処理

  1. customThe reaction
  2. temperaturevial was cooled to RT
  3. concentrationconcentrated on the rotary evaporator
  4. customwater (50 mL) the organic layer was separated
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. concentrationconcentrated
  7. customto yield the crude product which
  8. customwas purified by silica gel flash column chromatography (
  9. washeluted
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-103aa626ae2b4d49b14d6fc254007bf4
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08426447B2

反応ノート

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