Methanol → 1-Benzothiazol-6-yl-3-(2-chloro-1,1-dimethyl-ethyl)-urea

HRID 80214

반응식

HRID 80214 반응식
[S:1]1[C:5]2[CH:6]=[C:7]([NH2:10])[CH:8]=[CH:9][C:4]=2[N:3]=[CH:2]1.[Cl:11][CH2:12][C:13]([N:16]=[C:17]=[O:18])([CH3:15])[CH3:14].CO>C1(C)C=CC=CC=1.C(Cl)(Cl)Cl>[S:1]1[C:5]2[CH:6]=[C:7]([NH:10][C:17]([NH:16][C:13]([CH3:15])([CH3:14])[CH2:12][Cl:11])=[O:18])[CH:8]=[CH:9][C:4]=2[N:3]=[CH:2]1

참가 물질

6

반응물 3

HCID 887MethanolHCID 682886-AminobenzothiazoleHCID 110407471-Chloro-2-isocyanato-2-methyl-propane

생성물 1

HCID 687898531-Benzothiazol-6-yl-3-(2-chloro-1,1-dimethyl-ethyl)-urea수율 18.5%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6212Chloroform용매

실험 절차

Benzothiazol-6-ylamine (1.8 g, 12.00 mmol) was added portion wise to solution of 1-chloro-2-isocyanato-2-methyl-propane (2 g, 13.60 mmol) in toluene (20 mL) over a period of 5 minutes. The resulting mixture was stirred at room temperature for 2½ days. The reaction was monitored by TLC (5% MeOH in CHCl3). The reaction mixture was concentrated and extracted with ethylacetate. The organic layer was dried over Na2SO4 and concentrated. Purification by column chromatography on silica gel (1% MeOH in CHCl3) afforded 630 mg of the product (16.57% yield).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. extractionextracted with ethylacetate
  3. dry with materialThe organic layer was dried over Na2SO4
  4. concentrationconcentrated
  5. customPurification by column chromatography on silica gel (1% MeOH in CHCl3)

출처 및 근거

ORD 기록
ord-7d4430f7215241d5bbc8a1235cd54f54
출처 데이터셋
uspto-grants-2014_09
특허 번호
USRE045173E1

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