p-Toluenesulfonic acid → HCID 59075103、化合物

HRID 712809ノート

反応式

HRID 712809 の反応式
CC1(C)[N:6]2[C:7](=[O:12])[C:8]([CH3:11])([CH3:10])[CH2:9][C@@H:5]2[CH2:4][O:3]1.CC1C=CC(S(O)(=O)=O)=CC=1>CO>[OH:3][CH2:4][C@@H:5]1[NH:6][C:7](=[O:12])[C:8]([CH3:11])([CH3:10])[CH2:9]1

参加物

4

反応物 2

HCID 6101p-Toluenesulfonic acidHCID 89370059(7aR)-Tetrahydro-3,3,6,6-tetramethyl-3H,5H-pyrrolo[1,2-c]oxazol-5-one

生成物 1

HCID 59075103HCID 59075103、化合物収率 123.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a stirred suspension of (R)-3,3,6,6-tetramethyltetrahydropyrrolo[1,2-c]oxazol-5(3H)-one (D35) (714 mg, 3.89 mmol) in MeOH (15 ml), p-TSA (74 mg, 0.39 mmol) was added and the resulting mixture was heated at reflux for 2 hrs. Solvent was evaporated off and the residue was loaded on SPE-SCX cartridge (5 g). The cartridge was washed with MeOH (3 column volume). The methanolic phase was collected and evaporated to afford the title compound (D36) (690 mg)

後処理

  1. additionwas added
  2. temperaturethe resulting mixture was heated
  3. temperatureat reflux for 2 hrs
  4. customSolvent was evaporated off
  5. washThe cartridge was washed with MeOH (3 column volume)
  6. customThe methanolic phase was collected
  7. customevaporated

出典と根拠

ORDレコード
ord-8becd33ec58c4b2ea15da42d5be9b3ac
出典データセット
uspto-grants-2015_11
特許番号
US09181279B2

反応ノート

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