Sodium Nitrite → HCID 178515102、化合物

HRID 1043454ノート

反応式

HRID 1043454 の反応式
[N:1]([O-:3])=O.[Na+].[N:5]1[C:10]2[NH:11][C:12]3[CH:20]=[N:19][CH:18]=[CH:17][C:13]=3[CH2:14][C:15](=[O:16])[C:9]=2[CH:8]=[CH:7][CH:6]=1>O.C(O)(=O)C>[NH:5]1[C:10]2=[N:11][C:12]3[CH:20]=[N:19][CH:18]=[CH:17][C:13]=3/[C:14](=[N:1]/[OH:3])/[C:15](=[O:16])[C:9]2=[CH:8][CH:7]=[CH:6]1

参加物

5

反応物 2

HCID 23668193Sodium NitriteHCID 547591456,11-dihydro-5H-dipyrido[2,3-b:4',3'-f]azepin-5-one

生成物 1

HCID 178515102HCID 178515102、化合物収率 87%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒2 回

実験手順

A solution of sodium nitrite (3.3 g, 0.048 mol) in water (14.4 mL) was added dropwise to a solution of 6,11-dihydro-5H-dipyrido[2,3-b:4′,3′-f]azepin-5-one (4.22 g, 0.02 mol) in acetic acid (80 mL) at room temperature. After the addition was completed, the reaction was stirred for 1.5 hours and 100 mL of water was then added. The mixture was stirred for additional 10 minutes, filtered and dried to give 4.18 g of the desired product. 1H NMR (400 MHz, CD3OD): δ 8.70 (s, 1H), 8.48-8.51 (m, 2H), 8.32 (d, 1H, J=5.2 Hz), 7.56 (d, 1H, J=5.6 Hz), 7.07 (dd, 1H, J1=8 Hz, J2=4.8 Hz). MS [M+H]=241.

後処理

  1. additionAfter the addition
  2. stirringThe mixture was stirred for additional 10 minutes
  3. filtrationfiltered
  4. customdried

出典と根拠

ORDレコード
ord-15b3be77e53b45b2b84d3fef6f2ae04a
出典データセット
uspto-grants-2013_10
特許番号
US08563541B2

反応ノート

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