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4-Methyl-5-(2-hydroxyethyl)thiazole → 103871-46-1

HRID 1684641
ノート
印刷プレビュー

反応式

HRID 1684641 の反応式
[OH:1][CH2:2][CH2:3][C:4]1[S:8][CH:7]=[N:6][C:5]=1[CH3:9].[Br:10][CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13]>C(O)C>[Br-:10].[CH2:15]([O:14][C:12]([CH2:11][N+:6]1[C:5]([CH3:9])=[C:4]([CH2:3][CH2:2][OH:1])[S:8][CH:7]=1)=[O:13])[CH3:16]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 11364-Methyl-5-(2-hydroxyethyl)thiazoleHCID 7748Ethyl bromoacetate

生成物 1

HCID 10935796103871-46-1収率 71.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
0 °C

実験手順

A solution of 5-(2-hydroxyethyl)-4-methylthiazole (306 g) and ethyl bromoacetate (356.2 g) in ethanol (1 L) was heated to reflux. After two hours, the ethanol was removed by distillation and the residue treated with isopropanol (1.5 L). The resulting solution was cooled to about 0° C., causing crystallization of compound 1. After three hours, the crystalline material was separated from the mother liquor. Additional crystals were obtained by prolonged cooling of the mother liquor at 0° C. Combination of the crystalline material gave 474.3 g of compound 1. Melting point 96°-98° C.

後処理

  1. customthe ethanol was removed by distillation
  2. additionthe residue treated with isopropanol (1.5 L)
  3. customcrystallization of compound 1
  4. waitAfter three hours
  5. customthe crystalline material was separated from the mother liquor
  6. customAdditional crystals were obtained
  7. temperatureby prolonged cooling of the mother liquor at 0° C

出典と根拠

ORDレコード
ord-ec0ef138885940ce878ddf63f1ebc86d
出典データセット
uspto-grants-1997_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05641798

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート