Acetic Acid → 7-Amino-4-benzyloxy-1,2-benzisothiazole

HRID 1449120노트

반응식

HRID 1449120 반응식
[N+:1]([C:4]1[C:12]2[S:11][N:10]=[CH:9][C:8]=2[C:7]([O:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[CH:6][CH:5]=1)([O-])=O.O.C(O)(=O)C.N>[Fe].C(O)CC>[NH2:1][C:4]1[C:12]2[S:11][N:10]=[CH:9][C:8]=2[C:7]([O:13][CH2:14][C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)=[CH:6][CH:5]=1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 222AmmoniaHCID 962WaterHCID 203499427-Nitro-4-benzyloxy-1,2-benzisothiazole

생성물 1

HCID 203499357-Amino-4-benzyloxy-1,2-benzisothiazole수율 100%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 10311-Propanol용매

실험 절차

28.6 g of 7-nitro-4-benzyloxy-1,2-benzisothiazole are added in portions to a boiling mixture of 67 ml of water, 30 g of iron powder, 3 ml of glacial acetic acid and 167 ml of n-propanol and the mixture is then refluxed for a further hour. When it has cooled, it is neutralized with concentrated ammonia solution and filtered. The filter residue is washed with methylene chloride and the combined wash solutions are dried over magnesium sulfate and freed from the solvent under reduced pressure. 25.1 g (100% of theory) of 7-amino-4-benzyloxy-1,2-benzisothiazole of melting point 126°-128° C. are obtained.

후처리

  1. temperaturethe mixture is then refluxed for a further hour
  2. temperatureWhen it has cooled
  3. filtrationfiltered
  4. washThe filter residue is washed with methylene chloride
  5. dry with materialthe combined wash solutions are dried over magnesium sulfate

출처 및 근거

ORD 기록
ord-d0ff86413b954b0d97b5004a7967a224
출처 데이터셋
uspto-grants-1980_02
특허 번호
US04189433

반응 노트

불러오는 중…