Water → HCID 86732632、化合物

HRID 626393ノート

反応式

HRID 626393 の反応式
CC1C=CC(S(O[CH2:12][CH2:13][C@H:14]2[CH2:17][CH2:16][O:15]2)(=O)=O)=CC=1.[N-:18]=[N+:19]=[N-:20].[Na+].O>CS(C)=O>[N:18]([CH2:12][CH2:13][C@H:14]1[CH2:17][CH2:16][O:15]1)=[N+:19]=[N-:20]

参加物

5

反応物 3

HCID 962WaterHCID 33557Sodium AzideHCID 86732633HCID 86732633、化合物

生成物 1

HCID 86732632HCID 86732632、化合物

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
55 °C

実験手順

The mixture of (R)-2-(oxetan-2-yl)ethyl 4-methylbenzenesulfonate (80 mg, 0.31 mmol), NaN3 (30 m2, 0.465 mmol) and KI (5 mg) in DMSO (1 mL) was heated to 55° C. and stirred for 18 h. Then the mixture was cooled to RT, then it was poured into 20 mL of water, then extracted with MTBE (20 mL×3), the organic layers was washed with 1-120 (10 mL), brine (10 mL), and dried over Na2SO4. After filtration, the filtrate was concentrated under the reduced pressure. to give the titled compound which was used to the next step without further purification.

後処理

  1. temperatureThen the mixture was cooled to RT
  2. extractionextracted with MTBE (20 mL×3)
  3. washthe organic layers was washed with 1-120 (10 mL), brine (10 mL)
  4. dry with materialdried over Na2SO4
  5. filtrationAfter filtration
  6. concentrationthe filtrate was concentrated under the reduced pressure

出典と根拠

ORDレコード
ord-3cd014bad5fc4d2fa9dc946c3275d6de
出典データセット
uspto-grants-2016_04
特許番号
US09309227B2

反応ノート

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