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

HRID 1579242노트

반응식

HRID 1579242 반응식
[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

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

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 for up to 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.

후처리

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

출처 및 근거

ORD 기록
ord-4ca80b449de04829b99e2a9ebc4ed06c
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03931179

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