Hydrochloric Acid → HCID 54054669、化合物

HRID 987306ノート

反応式

HRID 987306 の反応式
C(N(CC)CC)C.[CH3:8][S:9](Cl)(=[O:11])=[O:10].[CH2:13]([O:15][C:16](=[O:38])[CH:17]([O:35][CH2:36][CH3:37])[CH2:18][C:19]1[CH:24]=[CH:23][C:22]([O:25][CH2:26][CH2:27][C:28]2[CH:33]=[CH:32][C:31]([NH2:34])=[CH:30][CH:29]=2)=[CH:21][CH:20]=1)[CH3:14].Cl>ClCCl>[CH2:13]([O:15][C:16](=[O:38])[CH:17]([O:35][CH2:36][CH3:37])[CH2:18][C:19]1[CH:24]=[CH:23][C:22]([O:25][CH2:26][CH2:27][C:28]2[CH:29]=[CH:30][C:31]([NH:34][S:9]([CH3:8])(=[O:11])=[O:10])=[CH:32][CH:33]=2)=[CH:21][CH:20]=1)[CH3:14]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 53920635HCID 53920635、化合物

生成物 1

HCID 54054669HCID 54054669、化合物収率 72%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Triethylamine (0.544 g; 2.99 mmole) and thereafter methanesulfonyl chloride (0.392 g; 2.99 mmole) were added to a solution of 3-{4-[2-(4-aminophenyl)ethoxy]phenyl}-2-ethoxypropanoic acid ethyl ester (0.89 g; 2.49 mmole) in dichloromethane (8.9 ml) at 0° C. After stirring at room temperature for 20 hours the reaction mixture was poured onto a mixture of hydrochloric acid and ice. Dichloromethane was added, the phases were separated and the organic phase was washed with water, dried (sodium sulfate), filtered and the solvent was evaporated in vacuo. Purification by chromatography on silica gel using heptane:ethyl acetate (3:2) as eluant gave 0.78 g (yield 72%) of 2-ethoxy-3-{4-[2-(4-methanesulfonylaminophenyl)ethoxy]phenyl}propanoic acid ethyl ester.

後処理

  1. customthe phases were separated
  2. washthe organic phase was washed with water
  3. dry with materialdried (sodium sulfate)
  4. filtrationfiltered
  5. customthe solvent was evaporated in vacuo
  6. customPurification by chromatography on silica gel

出典と根拠

ORDレコード
ord-0bd7edbde247463398aec250d160fa0d
出典データセット
uspto-grants-2003_10
特許番号
US06630600B1

反応ノート

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