p-Toluenesulfonic acid → HCID 59075103, 화합물

HRID 712809노트

반응식

HRID 712809 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 59075103HCID 59075103, 화합물수율 123.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-8becd33ec58c4b2ea15da42d5be9b3ac
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181279B2

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