Pyridine → HCID 86736632, 화합물

HRID 1855829노트

반응식

HRID 1855829 반응식
[OH:1][CH2:2][C@@H:3]1[C@@H:8]([CH2:9][OH:10])[CH:7]2[CH2:11][CH:4]1[CH2:5][CH2:6]2.N1C=CC=CC=1.[C:18]1([CH3:28])[CH:23]=[CH:22][C:21]([S:24](Cl)(=[O:26])=[O:25])=[CH:20][CH:19]=1>O>[S:24]([C:21]1[CH:22]=[CH:23][C:18]([CH3:28])=[CH:19][CH:20]=1)([OH:1])(=[O:26])=[O:25].[S:24]([C:21]1[CH:22]=[CH:23][C:18]([CH3:28])=[CH:19][CH:20]=1)([OH:1])(=[O:26])=[O:25].[OH:1][CH2:2][C@@H:3]1[C@@H:8]([CH2:9][OH:10])[CH:7]2[CH2:11][CH:4]1[CH2:5][CH2:6]2

참가 물질

5

반응물 3

HCID 1049PyridineHCID 73974-Toluenesulfonyl chlorideHCID 57246542HCID 57246542, 화합물

생성물 1

HCID 86736632HCID 86736632, 화합물수율 223.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

In a 200 ml round bottom flask capped with a CaCl2 drying tube was placed 7.2 g (0.0461 moles) of (2S,3S)-2,3-bis(hydroxymethyl)bicyclo[2.2.1]heptane (m.p. 58° C.) together with 45 ml of pyridine and 18.4 g (0.096 moles) of p-toluenesulfonyl chloride. The mixture was cooled in an ice bath and stirred for 3 hours and then diluted with 10 ml of H2O. The precipitate which formed was filtered and washed to remove pyridine. The solid was recrystallized from ethanol to give 17.2 g (92%) of fine white needles, m.p. 100°-101° C., αD =+32.2° C.

후처리

  1. customIn a 200 ml round bottom flask capped with a CaCl2 drying tube
  2. temperatureThe mixture was cooled in an ice bath
  3. customThe precipitate which formed
  4. filtrationwas filtered
  5. washwashed
  6. customto remove pyridine
  7. customThe solid was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-e93c5cb704984e3a97d0affec8c71bb9
출처 데이터셋
uspto-grants-1980_08
특허 번호
US04216331

반응 노트

불러오는 중…