Triethylamine → HCID 13884647, 화합물

HRID 236047노트

반응식

HRID 236047 반응식
[C:1]1([C:7]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[S:8][CH2:9][CH2:10][OH:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:24][S:25](Cl)(=[O:27])=[O:26].C(N(CC)CC)C>ClCCl>[CH3:24][S:25]([O:11][CH2:10][CH2:9][S:8][C:7]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)([C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1)[C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)(=[O:27])=[O:26]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 2793702-(tritylsulfanyl)ethanol

생성물 1

HCID 13884647HCID 13884647, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 2-(triphenylmethylthio)ethanol (2.66 g, 8.30 mmol) in cold (0° C.) dichloromethane (39 mL) kept under a nitrogen atmosphere was added methanesulfonyl chloride (0.704 mL, 9.10 mmol); the resulting mixture was treated dropwise (15 min) with triethylamine (1.34 mL, 9.6 mmol). After stirring for 15 min, the cooling bath was removed and the reaction mixture was stirred for 7 h then washed successively with water (10 mL), 0.5N citric acid (10 mL), water (10 mL), saturated sodium bicarbonate and water. The organic extracts were dried (MgSO4 -MgO) and concentrated under reduced pressure to a thick syrup which crystallized on standing. Trituration of the crystals in ether afforded white solid 2.1 g (63%) mp 95°-8° C.; ir (KBr) νmax : 1580, 1565 (phenyl), 1350, 1175, 1165 cm-1 (sulfonate); 1Hmr (CDCl3): 2.51 (2H, t, J=6.6 Hz, CH2S), 3.07 (3H, s, CH3SO3-), 3.87 (2H, t, J=6.6 Hz, CH2O), 7.34 (15H, m, phenyl).

후처리

  1. customthe cooling bath was removed
  2. stirringthe reaction mixture was stirred for 7 h
  3. washthen washed successively with water (10 mL), 0.5N citric acid (10 mL), water (10 mL), saturated sodium bicarbonate and water
  4. dry with materialThe organic extracts were dried (MgSO4 -MgO)
  5. concentrationconcentrated under reduced pressure to a thick syrup which
  6. customcrystallized

출처 및 근거

ORD 기록
ord-9c102738d43d4b81b7b507406f5b87ba
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04642341

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