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

HRID 1449120ノート

反応式

HRID 1449120 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 203499357-Amino-4-benzyloxy-1,2-benzisothiazole収率 100%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 10311-Propanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d0ff86413b954b0d97b5004a7967a224
出典データセット
uspto-grants-1980_02
特許番号
US04189433

反応ノート

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