4-Methyl-5-(2-hydroxyethyl)thiazole → HCID 21299287, 화합물

HRID 259665

반응식

HRID 259665 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 21299287HCID 21299287, 화합물수율 82%

시약·촉매·용매 2

HCID 7108Phenothiazine촉매HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8627cfb12c4d4690b5b4114f3be7f363
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05523152

연결된 노트

불러오는 중…