Methyl 7-Nitro-1,4-benzodioxane-6-carboxylate → Methyl 7-amino-2,3-dihydro-1,4-benzodioxin-6-carboxylate

HRID 596604ノート

反応式

HRID 596604 の反応式
[CH3:1][O:2][C:3](=[O:17])[C:4]1[C:9]([N+:10]([O-])=O)=[CH:8][C:7]2[O:13][CH2:14][CH2:15][O:16][C:6]=2[CH:5]=1>[Pd].C(O)(=O)C>[CH3:1][O:2][C:3](=[O:17])[C:4]1[C:9]([NH2:10])=[CH:8][C:7]2[O:13][CH2:14][CH2:15][O:16][C:6]=2[CH:5]=1

参加物

4

反応物 1

HCID 10537941Methyl 7-Nitro-1,4-benzodioxane-6-carboxylate

生成物 1

HCID 3146109Methyl 7-amino-2,3-dihydro-1,4-benzodioxin-6-carboxylate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

A mixture of 6.0 g. of 6-nitro-3,4-ethylenedioxybenzoic acid methyl ester, 150 mg. of 5% palladium on charcoal and 20 mls. of glacial acetic acid is hydrogenated under an initial hydrogen pressure of 30-40 p.s.i. and without external heating. After four hours the reaction mixture is filtered diluted with 80 ml. of ice water, stirred up one half hour and the resulting precipitate filtered off, water washed and dried to obtain 6-amino-3,4-ethylenedioxybenzoic acid methyl ester, m.p. 73°-77° C.

後処理

  1. additionA mixture of 6.0 g
  2. filtrationAfter four hours the reaction mixture is filtered
  3. additiondiluted with 80 ml
  4. filtrationthe resulting precipitate filtered off
  5. washwater washed
  6. customdried

出典と根拠

ORDレコード
ord-f940b815c6d64281b0e557a1548047c4
出典データセット
uspto-grants-1977_03
特許番号
US04011323

反応ノート

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