2-Methylbenzothiazole → Benzothiazolium, 3-(2-hydroxyethyl)-2-methyl-, bromide (1:1)

HRID 1266948노트

반응식

HRID 1266948 반응식
[CH3:1][C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[Br:11][CH2:12][CH2:13][OH:14]>C(OCC)(=O)C>[Br-:11].[OH:14][CH2:13][CH2:12][N+:6]1[C:5]2[CH:7]=[CH:8][CH:9]=[CH:10][C:4]=2[S:3][C:2]=1[CH3:1]

참가 물질

4

반응물 2

HCID 84462-MethylbenzothiazoleHCID 108982-Bromoethanol

생성물 1

HCID 113017Benzothiazolium, 3-(2-hydroxyethyl)-2-methyl-, bromide (1:1)수율 39%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
110 °C

실험 절차

A solution of 2-methylbenzothiazole (5.87 g) and 2-bromoethanol (49.2 g) was stirred and heated in an oil bath at 110° C. for 18 hours. After cooling the reaction mixture to room temperature, adding ethyl acetate (100 ml), and decanting, the resultant solid was then dissolved in methanol (50 ml) and precipitated with ethyl acetate (300 ml). The solid was again recrystallized from a mixture of methanol and ethyl acetate, washed with ethyl acetate (2×25 ml) and dried in an oven under high vacuum at 50° C. overnight to obtain 4.21 g (39%) of 4a.

후처리

  1. temperatureAfter cooling the reaction mixture to room temperature
  2. customdecanting
  3. dissolutionthe resultant solid was then dissolved in methanol (50 ml)
  4. customprecipitated with ethyl acetate (300 ml)
  5. customThe solid was again recrystallized from a mixture of methanol and ethyl acetate
  6. washwashed with ethyl acetate (2×25 ml)
  7. customdried in an oven under high vacuum at 50° C. overnight

출처 및 근거

ORD 기록
ord-35379bfe34664ac48d3466f65a4d96bc
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06551831B2

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