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Triethylamine → ethyl N-(4-p-nitrophenyl-2-thiazolyl)carbamate

HRID 1980824
ノート
印刷プレビュー

反応式

HRID 1980824 の反応式
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[CH:9][CH:8]=2)[N:6]=1.C(N(CC)CC)C.Cl[C:24]([O:26][CH2:27][CH3:28])=[O:25]>O1CCCC1>[N+:13]([C:10]1[CH:9]=[CH:8][C:7]([C:5]2[N:6]=[C:2]([NH:1][C:24](=[O:25])[O:26][CH2:27][CH3:28])[S:3][CH:4]=2)=[CH:12][CH:11]=1)([O-:15])=[O:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 164202-Amino-4-(p-nitrophenyl)thiazole

生成物 1

HCID 5108134ethyl N-(4-p-nitrophenyl-2-thiazolyl)carbamate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

In 300 ml of tetrahydrofuran, was suspended 4.42 g of 2-amino-4-p-nitrophenylthiazole, followed by a further addition of 20 ml of triethylamine. The mixture was cooled to about 5° C., to which 10.5 ml of ethyl chloroformate was added dropwise. Then, the reaction mixture was stirred at room temperature for 3.5 days. Any insoluble matter was filtered off from the reaction mixture, and the filtrate was concentrated and then washed in ethyl acetate successively with water, dilute hydrochloric acid, and water. Then, the ethyl acetate solution was concentrated to about 50 ml and the resulting crystals were separated by filtration and then subjected to column chromatography on silica gel. The reaction product was eluted with a benzene/ethyl acetate mixed solvent. The resultant product was recrystallized from ethyl acetate to obtain 2.8 g of ethyl N-(4-p-nitrophenyl-2-thiazolyl)carbamate.

後処理

  1. additionwas added dropwise
  2. filtrationAny insoluble matter was filtered off from the reaction mixture
  3. concentrationthe filtrate was concentrated
  4. washwashed in ethyl acetate successively with water, dilute hydrochloric acid, and water
  5. concentrationThen, the ethyl acetate solution was concentrated to about 50 ml
  6. customthe resulting crystals were separated by filtration
  7. washThe reaction product was eluted with a benzene/ethyl acetate mixed solvent
  8. customThe resultant product was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-996f90971ad7454daceed7c35a8d519d
出典データセット
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04511574

反応ノート

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