1-Phenethylamine, (-)- → HCID 178462014、化合物

HRID 539611ノート

反応式

HRID 539611 の反応式
FC1C=CC=C(F)C=1O[C:5]1[O:6][C:7]([CH3:16])([CH3:15])[C:8]([CH3:14])([CH3:13])[S:9](=[O:12])(=[O:11])[N:10]=1.[C:22]1([C@@H:28]([NH2:30])[CH3:29])[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>>[C:22]1([C@@H:28]([NH:30][C:5]2[O:6][C:7]([CH3:15])([CH3:16])[C:8]([CH3:13])([CH3:14])[S:9](=[O:11])(=[O:12])[N:10]=2)[CH3:29])[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1

参加物

3

反応物 2

HCID 758181-Phenethylamine, (-)-HCID 867054542-(2,6-Difluorophenoxy)-5,5,6,6-tetramethyl-5,6-dihydro-1,4,3-oxathiazine 4,4-dioxide

生成物 1

HCID 178462014HCID 178462014、化合物収率 50.9%

実験手順

A mixture of 194 mg of 2-(2,6-difluorophenoxy)-5,5,6,6-tetramethyl-5,6-dihydro-1,4,3-oxathiazine 4,4-dioxide and 737 mg of (S)-1-phenylethylamine was stirred at room temperature for 16 hours and then purified in a purification laboratory by means of preparative HPLC. The combined product-containing fractions were alkalized with 25% aqueous ammonia solution and extracted three times with 30 ml of ethyl acetate, and the combined organic phases were dried over MgSO4 and concentrated by rotary evaporation. This gave the product (96 mg) with a molecular weight of 310.4 g/mol (C15H22N2O3S); MS (ESI): m/e=311 (M+H+).

後処理

  1. custompurified in a purification laboratory by means of preparative HPLC
  2. additionThe combined product-containing fractions
  3. extractionextracted three times with 30 ml of ethyl acetate
  4. dry with materialthe combined organic phases were dried over MgSO4
  5. concentrationconcentrated by rotary evaporation

出典と根拠

ORDレコード
ord-da46496f2c4848c3b900356353f84c50
出典データセット
uspto-grants-2014_10
特許番号
US08871758B2

反応ノート

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