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Triethylamine → HCID 66968183、化合物

HRID 549334
ノート
印刷プレビュー

反応式

HRID 549334 の反応式
[CH2:1]([O:3][C:4](=[O:12])[CH2:5][CH:6]1[CH2:11][O:10][CH2:9][CH2:8][NH:7]1)[CH3:2].C(N(CC)CC)C.[F:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]2[S:31][C:30]([CH3:32])=[N:29][C:28]=2[C:33](Cl)=[O:34])=[CH:23][CH:22]=1>ClCCl.O>[CH2:1]([O:3][C:4](=[O:12])[CH2:5][CH:6]1[CH2:11][O:10][CH2:9][CH2:8][N:7]1[C:33]([C:28]1[N:29]=[C:30]([CH3:32])[S:31][C:27]=1[C:24]1[CH:25]=[CH:26][C:21]([F:20])=[CH:22][CH:23]=1)=[O:34])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8471TriethylamineHCID 11789040Ethyl 2-(morpholin-3-yl)acetateHCID 223241192-Methyl-5-(4-fluorophenyl)thiazole-4-carbonyl chloride

生成物 1

HCID 66968183HCID 66968183、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

Morpholin-3-ylacetic acid ethyl ester Chem Pharm Bull 94, 31(1), 1983 (2.10 g) was dissolved in dichloromethane (50 ml) and treated with triethylamine (1.33 g). The mixture was cooled (ice bath) and 5-(4-fluoro-phenyl)-2-methyl-thiazole-4-carbonyl chloride (1.53 g) in dichloromethane (10 ml) added. The mixture was stirred for 16 h, diluted with water and the organic phase separated. The aqueous phase was extracted with dichloromethane (2×100 ml), the organic phases combined, dried (Na2SO4) and solvent removed at reduced pressure. the residue was column chromatographed (silica gel, 40% ethyl acetate:pentane ˜60% ethyl acetate pentane eluant) to give the title compound (1.46 g).

後処理

  1. additionadded
  2. customthe organic phase separated
  3. extractionThe aqueous phase was extracted with dichloromethane (2×100 ml)
  4. dry with materialdried (Na2SO4) and solvent
  5. customremoved at reduced pressure
  6. customchromatographed (silica gel, 40% ethyl acetate:pentane ˜60% ethyl acetate pentane eluant)

出典と根拠

ORDレコード
ord-39468204f0c949e6b1e9896f708fdab9
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07943645B2

反応ノート

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