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Methanesulfonamide → N-(4-hexadecylamino-2-thiophenecarbonyl)methanesulfonamide

HRID 850990
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HRID 850990 반응식
Cl.[CH2:2]([NH:18][C:19]1[CH:20]=[C:21]([C:24](Cl)=[O:25])[S:22][CH:23]=1)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17].[CH3:27][S:28]([NH2:31])(=[O:30])=[O:29]>N1C=CC=CC=1>[CH2:2]([NH:18][C:19]1[CH:20]=[C:21]([C:24]([NH:31][S:28]([CH3:27])(=[O:30])=[O:29])=[O:25])[S:22][CH:23]=1)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 72879MethanesulfonamideHCID 205036504-Hexadecylamino-2-thiophenecarbonyl chloride hydrochloride

생성물 1

HCID 20503666N-(4-hexadecylamino-2-thiophenecarbonyl)methanesulfonamide

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A solution of 25 g. of 4-hexadecylamino-2-thiophenecarbonyl chloride hydrochloride and 5.6 g. of methanesulfonamide in 250 ml. of pyridine is stirred under reflux for 2 hours and then concentrated in vacuo. The residue is partitioned between water and diethyl ether; the aqueous layer acidified with 1 N hydrochloric acid and the organic layer seperated, dried over magnesium sulfate, and evaporated. Crystallization of the residual white solid from 60% aqueous acetic acid and then from methylene chloride-hexane affords the product as a white solid.

후처리

  1. temperatureunder reflux for 2 hours
  2. concentrationconcentrated in vacuo
  3. customThe residue is partitioned between water and diethyl ether
  4. customthe organic layer seperated
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customCrystallization of the residual white solid from 60% aqueous acetic acid

출처 및 근거

ORD 기록
ord-9a5bd030495b4dbdb529cc933f2f50ca
출처 데이터셋
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04382143

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