Triethylamine → Methyl 2-methanesulfonyl-3-phenylbenzoate

HRID 1764450ノート

反応式

HRID 1764450 の反応式
O[C:2]1[C:11]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].[CH3:18][S:19](Cl)(=[O:21])=[O:20].CCN(CC)CC>>[CH3:18][S:19]([C:2]1[C:11]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5])(=[O:21])=[O:20]

参加物

4

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 241577Methyl 2-hydroxy-3-phenylbenzoate

生成物 1

HCID 22768433Methyl 2-methanesulfonyl-3-phenylbenzoate

実験手順

An ethereal solution (1 liter) containing 50.0 g (0.22 mol) of methyl 2-hydroxy-3-phenylbenzoate, 0.25 mole of methanesulfonyl chloride and 0.25 mole of Et3N was allowed to react at room temperature for 18 hours. The reaction mixture was washed with 1 N NaOH (1 × 1 liter) and H2O (1 × 500 ml). After drying with MgSO4 the ether solution was evaporated to give a yellow solid; yield 61.9 g (91.7%), mp. 101°-115°. Recrystallization of the crude product from benzene-hexane gave the analytical sample, mp. 120°-124°.

後処理

  1. customto react at room temperature for 18 hours
  2. washThe reaction mixture was washed with 1 N NaOH (1 × 1 liter) and H2O (1 × 500 ml)
  3. dry with materialAfter drying with MgSO4 the ether solution
  4. customwas evaporated
  5. customto give a yellow solid
  6. customRecrystallization of the crude product from benzene-hexane
  7. customgave the analytical sample, mp. 120°-124°

出典と根拠

ORDレコード
ord-96c52519c78046a097b6ecad7ca34539
出典データセット
uspto-grants-1978_09
特許番号
US04116961

反応ノート

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