4-Methyl-5-(2-hydroxyethyl)thiazole → HCID 21299287、化合物

HRID 259665

反応式

HRID 259665 の反応式
[OH:1][CH2:2][CH2:3][C:4]1[S:8][CH:7]=[N:6][C:5]=1[CH3:9].C(N(CC)CC)C.[C:17](Cl)(=[O:20])[CH:18]=[CH2:19]>C1C2NC3C(=CC=CC=3)SC=2C=CC=1.C(Cl)(Cl)Cl>[C:17]([O:1][CH2:2][CH2:3][C:4]1[S:8][CH:7]=[N:6][C:5]=1[CH3:9])(=[O:20])[CH:18]=[CH2:19]

参加物

6

反応物 3

HCID 11364-Methyl-5-(2-hydroxyethyl)thiazoleHCID 8471TriethylamineHCID 13140Acryloyl chloride

生成物 1

HCID 21299287HCID 21299287、化合物収率 82%

試薬・触媒・溶媒 2

HCID 7108Phenothiazine触媒HCID 6212Chloroform溶媒

実験手順

A one liter, three necked flask was equipped with overhead stirrer, nitrogen atmosphere and an addition funnel. The flask was charged with 100 g of 5-(2-hydroxyethyl)-4-methylthiazole (0.70 mol.), 71 g of triethylamine (0.70 mol.), 500 g of chloroform and 3 g of phenothiazine. Next, 63 g of acryloyl chloride (0.70 mol.) was slowly added to the reaction over 1.5 hour via the addition funnel. The reaction was stirred for 2 hours at room temperature. The reaction mixture was extracted with NaCl(aq.), NH4OH(10%), NaCl(aq.) and dried over MgSO4. The chloroform was evaporated with a rotoevaporator to yield 113 g (82%) of a dark brown liquid. The product was confirmed by IR and 13C NMR.

後処理

  1. customA one liter, three necked flask was equipped with overhead stirrer
  2. extractionThe reaction mixture was extracted with NaCl(aq.), NH4OH(10%), NaCl(aq.)
  3. dry with materialdried over MgSO4
  4. customThe chloroform was evaporated with a rotoevaporator

出典と根拠

ORDレコード
ord-8627cfb12c4d4690b5b4114f3be7f363
出典データセット
uspto-grants-1996_06
特許番号
US05523152

関連ノート

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