Triethylamine → HCID 86607107, 화합물

HRID 900883노트

반응식

HRID 900883 반응식
[NH2:1][CH:2]([CH2:5][OH:6])[CH2:3][OH:4].[C:7]([NH:10][C:11]1[S:12][C:13]([S:17](Cl)(=[O:19])=[O:18])=[C:14]([CH3:16])[N:15]=1)(=[O:9])[CH3:8].C(N(CC)CC)C>C1COCC1>[OH:4][CH2:3][CH:2]([NH:1][S:17]([C:13]1[S:12][C:11]([NH:10][C:7](=[O:9])[CH3:8])=[N:15][C:14]=1[CH3:16])(=[O:18])=[O:19])[CH2:5][OH:6]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 68294SerinolHCID 969512-Acetamido-4-methylthiazole-5-sulfonyl chloride

생성물 1

HCID 86607107HCID 86607107, 화합물수율 60.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of 2-amino-1,3-propanediol (2.15 g, 23.6 mmol) in THF (26 ml) was added at 0° C. (ice water bath) commercially available 2-acetamido-4-methylthiazole-5-sulfonyl chloride (2.0 g, 7.85 mmol) and triethylamine (1.2 ml, 8.64 mmol). The light yellow suspension was stirred at room temperature for 17 h, and evaporated. The crude product was further purified by column chromatography on silica gel (dichloromethane/MeOH/NH4OH 80:10:1) to yield 2-acetamido-4-methyl-thiazole-5-sulfonic acid (2-hydroxy-1-hydroxymethyl-ethyl)-amide (1.46 g, 60%) as a light yellow solid. MS (ISP) 308.1 [(M−H)−]; mp 217° C.

후처리

  1. customevaporated
  2. customThe crude product was further purified by column chromatography on silica gel (dichloromethane/MeOH/NH4OH 80:10:1)

출처 및 근거

ORD 기록
ord-299ccea4a13244a8b15997c147a2a91f
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07361659B2

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