Ethyl Acetate → 5-Bromopyridine-2,3-diamine

HRID 55501

反応式

HRID 55501 の反応式
[NH2:1][C:2]1[C:7]([N+:8]([O-])=O)=[CH:6][C:5]([Br:11])=[CH:4][N:3]=1.O.O.[Sn](Cl)Cl.[BH4-].[Na+].C(OCC)(=O)C>CC(O)(C)C>[Br:11][C:5]1[CH:6]=[C:7]([NH2:8])[C:2]([NH2:1])=[N:3][CH:4]=1

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 61436Stannous chloride dihydrateHCID 1388782-Amino-5-bromo-3-nitropyridineHCID 4311764Sodium borohydride

生成物 1

HCID 6911565-Bromopyridine-2,3-diamine

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

実験手順

A procedure similar to that described in Preparation 42 was repeated, except that 12.0 g of 2-amino-5-bromo-3-nitropyridine (prepared as described in Preparation 56), 62.1 g of tin(II) chloride dihydrate, 1.04 g of sodium borohydride and 300 ml of a 9:1 by volume mixture of ethyl acetate and 2-methyl-2-propanol were used, to give the title compound as a crude product. This crude product was crystallized by trituration with a mixture of ethyl acetate and hexane, to give 7.46 g of the title compound, melting at 135°-137° C.

後処理

  1. customA procedure similar to that described in Preparation 42

出典と根拠

ORDレコード
ord-e2de0ed915b2471ebddf711e17debd8c
出典データセット
uspto-grants-1997_04
特許番号
US05624935

関連ノート

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