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

HRID 1463429노트

반응식

HRID 1463429 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-40766786739948c1b0d8c48a9d74ced2
출처 데이터셋
uspto-grants-1994_04
특허 번호
US05300518

반응 노트

불러오는 중…