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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Water → HCID 20237819、化合物

HRID 365200
ノート
印刷プレビュー

反応式

HRID 365200 の反応式
[CH2:1]([O:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH:2]1[O:4][CH2:3]1.[CH3:12][O:13][C:14]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[C:17]([NH:24][CH2:25][CH2:26][NH2:27])=[N:16][CH:15]=1.O>CN(C)C=O>[O:5]([CH2:1][CH:2]([OH:4])[CH2:3][NH:27][CH2:26][CH2:25][NH:24][C:17]1[C:18]2[C:23](=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:14]([O:13][CH3:12])=[CH:15][N:16]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 31217Phenyl glycidyl etherHCID 202378914-Methoxy-1-(2-aminoethylamino)-isoquinoline

生成物 1

HCID 20237819HCID 20237819、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

5.2 g. Phenyl glycidyl ether and 15 g. 4-methoxy-1-(2-aminoethylamino)-isoquinoline are dissolved in dimethylformamide and left to stand for 72 hours at ambient temperature. The reaction mixture is then poured into water, extracted with methylene chloride, dried and purified chromatographically on a silica gel column using, as elution agent, methylene chloride-methanol-triethylamine (8:1:0.05 v/v/v). By evaporation of the pure fractions, there are obtained 5.5 g. (44% of theory) of an oil. By the addition of 1.7 g. fumaric acid to a solution of this oil in ethyl acetate-ethanol, a hydrogen fumarate is precipitated out and this is then recrystallized from isopropyl alcohol. The desired product is obtained in the form of colorless crystals; m.p. 152°-153° C.

後処理

  1. waitleft
  2. extractionextracted with methylene chloride
  3. customdried
  4. custompurified chromatographically on a silica gel column
  5. washusing, as elution agent, methylene chloride-methanol-triethylamine (8:1:0.05 v/v/v)
  6. customBy evaporation of the pure fractions, there
  7. customare obtained 5.5 g
  8. additionBy the addition of 1.7 g
  9. customfumaric acid to a solution of this oil in ethyl acetate-ethanol, a hydrogen fumarate is precipitated out
  10. customthis is then recrystallized from isopropyl alcohol

出典と根拠

ORDレコード
ord-3c6dcca7bea5418197b47c36421bae60
出典データセット
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04608383

反応ノート

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