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

HRID 1266954노트

반응식

HRID 1266954 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][CH:12]([OH:14])[CH3:13]>>[Br-:11].[OH:14][CH2:12][CH2:13][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

3

반응물 2

HCID 84462-MethylbenzothiazoleHCID 14202443Ethanol, 1-bromo-

생성물 1

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

실험 절차

A solution of 2-methylbenzothiazole (5.87 g) and bromoethanol (49.2 g) were stirred in an oil bath at 110° C. for 18 hours. Added ethyl acetate (100 mL) to the reaction mixture and decanted. The residual solid was then dissolved in methanol (50 mL) and precipitated with ethyl acetate (300 mL). The solid was again recrystallized from methanol-ethyl acetate (15 mL/150 mL), washed with ethyl acetate (2×25 mL) and dried in an oven under high vacuum at 50° C. overnight. The yield was 4.21 g (39%). TLC (silica gel, 4:1 methylene chloride-methanol) Rf=0.34.

후처리

  1. customAdded ethyl acetate (100 mL) to the reaction mixture and decanted
  2. dissolutionThe residual solid was then dissolved in methanol (50 mL)
  3. customprecipitated with ethyl acetate (300 mL)
  4. customThe solid was again recrystallized from methanol-ethyl acetate (15 mL/150 mL)
  5. washwashed with ethyl acetate (2×25 mL)
  6. customdried in an oven under high vacuum at 50° C. overnight

출처 및 근거

ORD 기록
ord-3996b4f376034c20a93a45a4cf215338
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06551831B2

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