Sodium Hydroxide → 2-Amino-6-methoxy-4,5,7-trimethylbenzothiazole

HRID 1463429ノート

反応式

HRID 1463429 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([O:9][CH3:10])=[C:4]([CH3:11])[C:3]=1[CH3:12].[S-:13][C:14]#[N:15].[K+].BrBr.[OH-].[Na+]>C(O)(=O)C.O>[NH2:15][C:14]1[S:13][C:7]2[C:6]([CH3:8])=[C:5]([O:9][CH3:10])[C:4]([CH3:11])=[C:3]([CH3:12])[C:2]=2[N:1]=1

参加物

7

反応物 4

HCID 14798Sodium HydroxideHCID 24408BromineHCID 516872Potassium thiocyanateHCID 147002344-Methoxy-2,3,5-trimethylaniline

生成物 1

HCID 147002352-Amino-6-methoxy-4,5,7-trimethylbenzothiazole収率 91.4%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

100 g of 1-amino-4-methoxy-2,3,5-trimethylbenzene was dissolved in 1,000 ml of acetic acid and 50 ml of water. Then 212 g of potassium thiocyanate was added to the solution at room temperature. The reaction mixture was cooled with ice and 37.5 ml of bromine was added dropwise thereto, followed by stirring for 30 minutes. The reaction mixture was neutralized with a 1N aqueous solution of sodium hydroxide. The insoluble matters thus formed were separated by filtering and washed with water. After recrystallizing from methanol/tetrahydrofuran, 123 g of the title compound was obtained.

後処理

  1. additionwas added dropwise
  2. customThe insoluble matters thus formed
  3. customwere separated
  4. filtrationby filtering
  5. washwashed with water
  6. customAfter recrystallizing from methanol/tetrahydrofuran

出典と根拠

ORDレコード
ord-40766786739948c1b0d8c48a9d74ced2
出典データセット
uspto-grants-1994_04
特許番号
US05300518

反応ノート

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