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HCID 15718785、化合物 → HCID 178488097、化合物

HRID 2166125
ノート
印刷プレビュー

反応式

HRID 2166125 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[NH:10][C:11]([NH:13][CH:14]1[CH2:19][CH2:18][N:17]([CH3:20])[CH2:16][CH2:15]1)=S>[Hg]=O.O1CCCC1>[CH3:9][O:8][C:5]1[CH:6]=[CH:7][C:2]2[NH:1][C:11]([NH:13][CH:14]3[CH2:19][CH2:18][N:17]([CH3:20])[CH2:16][CH2:15]3)=[N:10][C:3]=2[CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 15718785HCID 15718785、化合物

生成物 1

HCID 178488097HCID 178488097、化合物収率 100%

試薬・触媒・溶媒 2

HCID 30856Mercuric oxide触媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 44 parts of N-(2-amino-5-methoxyphenyl)-N'-(1-methyl-4-piperidinyl)thiourea, 38.9 parts of mercury(II) oxide and 270 parts of tetrahydrofuran was stirred and refluxed for 2 hours at reflux temperature. The reaction mixture was filtered while hot over diatomaceous earth and the filtrate was evaporated. The residue was purified by column chromatography over silica gel first using a mixture of trichloromethane and methanol (95:5 by volume) and then a mixture of trichloromethane and methanol, saturated with ammonia, (85:15 by volume) as eluents. The pure fractions were collected and the eluent was evaporated, yielding 50.5 parts (100%) of 5-methoxy-N-(1-methyl-4-piperidinyl)-1H-benzimidazol-2-amine as a residue (interm. 27).

後処理

  1. temperaturerefluxed for 2 hours
  2. temperatureat reflux temperature
  3. filtrationThe reaction mixture was filtered while hot over diatomaceous earth
  4. customthe filtrate was evaporated
  5. customThe residue was purified by column chromatography over silica gel
  6. additiona mixture of trichloromethane and methanol (95:5 by volume)
  7. additiona mixture of trichloromethane and methanol
  8. customThe pure fractions were collected
  9. customthe eluent was evaporated

出典と根拠

ORDレコード
ord-939f27ad240c45b5b49fdfa90f601f7b
出典データセット
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04943580

反応ノート

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