Acefylline → HCID 86734928、化合物

HRID 258811

反応式

HRID 258811 の反応式
[CH:1](=[C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11][CH2:10][NH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N:18]1([C:29](=[O:30])[C:28]2[N:27]([CH2:31][C:32]([OH:34])=[O:33])[CH:26]=[N:25][C:24]=2[N:22]([CH3:23])[C:20]1=[O:21])[CH3:19]>C(O)CC>[CH:1](=[C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11][CH2:10][NH2+:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1.[N:18]1([C:29](=[O:30])[C:28]2[N:27]([CH2:31][C:32]([O-:34])=[O:33])[CH:26]=[N:25][C:24]=2[N:22]([CH3:23])[C:20]1=[O:21])[CH3:19]

参加物

4

反応物 2

HCID 69550AcefyllineHCID 70634238HCID 70634238、化合物

生成物 1

HCID 86734928HCID 86734928、化合物収率 48%

試薬・触媒・溶媒 1

HCID 10311-Propanol溶媒

実験手順

2.21 g. (0.01 mole) of 1-benzal-1,2,3,4-tetrahydroisoquinoline and 2.38 g. (0.01 mole) of theophylline-7-acetic acid are dissolved under boiling in 25 ml. of n-propanol. The undissolved substances is filtered from the hot solution. The clear filtrate is crystallized while the mixture is cooled. The precipitated crystals are filtered out, covered with n-propanol and dried at room temperature. Thus 2.2 g. of 1-benzal-1,2,3,4-tetrahydroisoquinolinium-theophylline-7-acetate yield 48%) are obtained. Mp.: 168°-173° C. After recrystallization from a twofold amount of n-propanol the melting point was 195°-198° C.

後処理

  1. filtrationThe undissolved substances is filtered from the hot solution
  2. customThe clear filtrate is crystallized while the mixture
  3. temperatureis cooled
  4. filtrationThe precipitated crystals are filtered out
  5. customdried at room temperature

出典と根拠

ORDレコード
ord-d139aa97146b4758aebd90d098d8954c
出典データセット
uspto-grants-1977_07
特許番号
US04035366

関連ノート

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