Toluene → HCID 178517902、化合物

HRID 2072474ノート

反応式

HRID 2072474 の反応式
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][C:2]=1[CH2:11][N:12]1[CH2:20][CH2:19][C:15]([NH:21][C:22]2C=CC=CC=2)([C:16]([NH2:18])=[O:17])[CH2:14][CH2:13]1.C(OCC)(OCC)OCC.C1(C)C=CC=CC=1.[OH-].[NH4+]>C(O)(=O)C>[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][C:2]=1[CH2:11][N:12]1[CH2:13][CH2:14][C:15]2([NH:21][CH:22]=[N:18][C:16]2=[O:17])[CH2:19][CH2:20]1

参加物

6

反応物 4

HCID 1140TolueneHCID 14923Ammonium HydroxideHCID 31214Ethyl orthoformateHCID 214082231-[(3,4-Dihydro-2-naphthalenyl)methyl]-4-anilino isonipecotamide

生成物 1

HCID 178517902HCID 178517902、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 1-[(3,4-dihydro-2-naphthalenyl)methyl]-4-anilino isonipecotamide (6.0 g), triethyl orthoformate (3.0 g), toluene (30 ml), and glacial acetic acid (1.5 ml) is refluxed under nitrogen for 38 hours. The reaction mixture is cooled and poured into aqueous ammonium hydroxide. The organic layer is separated, dried, and concentrated to give the crude product. Digestion of this material with benzene followed by filtration and concentration of the organic solution yields the title compound.

後処理

  1. temperatureis refluxed under nitrogen for 38 hours
  2. temperatureThe reaction mixture is cooled
  3. customThe organic layer is separated
  4. customdried
  5. concentrationconcentrated
  6. customto give the crude product
  7. filtrationDigestion of this material with benzene followed by filtration and concentration of the organic solution

出典と根拠

ORDレコード
ord-ef88f300af0b4791a2a6a5332dce9a59
出典データセット
uspto-grants-1977_09
特許番号
US04051248

反応ノート

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