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Ammonia → 4'-Chloro-2-hydroxy-4-methoxy-benzophenone imine

HRID 66245
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인쇄 미리보기

반응식

HRID 66245 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][C:10]=2[OH:17])=[CH:4][CH:3]=1.[NH3:19]>CO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[NH:19])[C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][C:10]=2[OH:17])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 665574'-Chloro-2-hydroxy-4-methoxybenzophenone

생성물 1

HCID 1363884104'-Chloro-2-hydroxy-4-methoxy-benzophenone imine

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A suspension of 132 g. of 4'-chloro-2-hydroxy-4-methoxy-benzophenone in 500 ml. of methanol is cooled to -20° C. in a 2 l. shaking autoclave and treated with 120 ml. of liquid ammonia. The mixture is then shaken at 120° C. for 20 hours under a nitrogen atmosphere. After cooling, the yellow crude product is filtered off under suction and washed with a small amount of methanol. There is obtained 4'-chloro-2-hydroxy-4-methoxy-benzophenone imine, having a melting point of 210°-212° C., which can be used in the next step without further purification. An analytical sample is obtained by recrystallization from methanol and has a melting point of 212°-214° C.

후처리

  1. additionA suspension of 132 g
  2. additiontreated with 120 ml
  3. stirringThe mixture is then shaken at 120° C. for 20 hours under a nitrogen atmosphere
  4. temperatureAfter cooling
  5. filtrationthe yellow crude product is filtered off under suction
  6. washwashed with a small amount of methanol

출처 및 근거

ORD 기록
ord-93a629a00dce41f082b242c9d0bb50a8
출처 데이터셋
uspto-grants-1978_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04130717

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