1-Chloro-4-(chloromethyl)benzene → HCID 178509292, 화합물

HRID 259085

반응식

HRID 259085 반응식
[NH2:1][C:2]1[N:6]=[C:5]([SH:7])[NH:4][N:3]=1.[Cl:8][C:9]1[CH:16]=[CH:15][C:12]([CH2:13]Cl)=[CH:11][CH:10]=1>[OH-].[Na+].C(O)C>[NH2:1][C:2]1[N:6]=[C:5]([S:7][CH2:13][C:12]2[CH:15]=[CH:16][C:9]([Cl:8])=[CH:10][CH:11]=2)[NH:4][N:3]=1

참가 물질

5

반응물 2

HCID 77231-Chloro-4-(chloromethyl)benzeneHCID 1785092965-amino-1H-1,2,4-triazole-3-thiol2회

생성물 1

HCID 178509292HCID 178509292, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 14798Sodium Hydroxide용매

실험 절차

A mixture of 3-amino-5-mercapto-s-triazole (Compound 5) [4.64g; 40 mmoles] in 40 ml. of IN sodium hydroxide was stirred at room temperature while solution of p-chlorobenzylchloride [7.55g; 48 mmoles] in 80 ml of absolute ethanol was added. The mixture was then warmed to 70°-75° and stirred for 30 minutes. The amber colored solution was then evaporated to 40 ml at reduced pressure, diluted with 50 ml of water and chilled overnight. The crude product was separated by filtration, air dried, and recrystallized two times from chloroform to afford 4.3g (45%) of analytically pure product that had a melting point of 107°-8°.

후처리

  1. additionwas added
  2. temperatureThe mixture was then warmed to 70°-75°
  3. customThe amber colored solution was then evaporated to 40 ml at reduced pressure
  4. additiondiluted with 50 ml of water
  5. temperaturechilled overnight
  6. customThe crude product was separated by filtration, air
  7. customdried
  8. customrecrystallized two times from chloroform
  9. customto afford 4.3g (45%) of analytically pure product that

출처 및 근거

ORD 기록
ord-eb3a8c657c95425085bb668a31f5529f
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04036840

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