Acetic Acid → 3,4-Dichloro-5-methyl-N-(1-nitrosopiperidin-4-yl)-1H-pyrrole-2-carboxamide

HRID 2233874ノート

反応式

HRID 2233874 の反応式
[N:1]([O-:3])=O.[Na+].FC(F)(F)C([O-])=O.[Cl:12][C:13]1[C:17]([Cl:18])=[C:16]([CH3:19])[NH:15][C:14]=1[C:20]([NH:22][CH:23]1[CH2:28][CH2:27][NH2+:26][CH2:25][CH2:24]1)=[O:21].C(O)(=O)C>O.C(O)C.O>[Cl:12][C:13]1[C:17]([Cl:18])=[C:16]([CH3:19])[NH:15][C:14]=1[C:20]([NH:22][CH:23]1[CH2:28][CH2:27][N:26]([N:1]=[O:3])[CH2:25][CH2:24]1)=[O:21]

参加物

6

反応物 3

HCID 176Acetic AcidHCID 23668193Sodium NitriteHCID 685798674-{[(3,4-Dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidinium trifluoroacetate2 回

生成物 1

HCID 866082583,4-Dichloro-5-methyl-N-(1-nitrosopiperidin-4-yl)-1H-pyrrole-2-carboxamide

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 19096565Water ethanol溶媒

反応条件

温度
90 °C

実験手順

A solution of NaNO2 (1.7 g, 24.6 mmol) in 20 ml of water was added to a solution of 4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidinium trifluoroacetate (Intermediate 86; 4 g, 10.3 mmol) and 400 μl acetic acid in 60 ml of 1:1 EtOH—H2O. The mixture was heated to 90° C. for 1 hour. After cooling to room temperature, 200 ml of water was added. White solids were collected by filtration and dried in vacuo (2.8 g).

後処理

  1. temperatureAfter cooling to room temperature
  2. filtrationWhite solids were collected by filtration
  3. customdried in vacuo (2.8 g)

出典と根拠

ORDレコード
ord-df58e45c1d7c497faec733b0e8249d0d
出典データセット
uspto-grants-2010_05
特許番号
US07709503B2

反応ノート

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