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

HRID 80274

反応式

HRID 80274 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6212Chloroform溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-8501abe5c47840b283062d540166e7c2
出典データセット
uspto-grants-2014_09
特許番号
USRE045173E1

関連ノート

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