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Formamidine acetate → HCID 13271775、化合物

HRID 464580
ノート
印刷プレビュー

反応式

HRID 464580 の反応式
C[O-].[Na+].C([O:8][C:9]([CH:11]1[C:17]2[CH:18]=[CH:19][C:20]([Cl:22])=[CH:21][C:16]=2[C:15]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[N:14][CH:13]=[CH:12]1)=O)CCC.C(OC(C1C2C=CC(Cl)=CC=2C(C2C=CC=CC=2)=NCC=1)=O)CCC.C(O)(=O)C.[CH:58]([NH2:60])=[NH:59]>C(O)C.O.CO>[Cl:22][C:20]1[CH:19]=[CH:18][C:17]2[CH:11]3[C:9](=[O:8])[NH:60][CH:58]=[N:59][CH:12]3[CH2:13][N:14]=[C:15]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[C:16]=2[CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 160693Formamidine acetateHCID 10942334Sodium MethoxideHCID 13271771Butyl 8-chloro-1-phenyl-3H-2-benzazepine-5-carboxylateHCID 13271773Butyl 8-chloro-1-phenyl-5H-2-benzazepine-5-carboxylate

生成物 1

HCID 13271775HCID 13271775、化合物

試薬・触媒・溶媒 3

HCID 702
Ethanol
溶媒
HCID 887Methanol溶媒
HCID 962Water溶媒

実験手順

Dropwise 9.5 mL (41 mmol) of a 4.3M methanol solution of sodium methoxide was added to a solution of 8.0 g (22.6 mmol) of a mixture of 8-chloro-1-phenyl-5H-2-benzazepine-5-carboxylic acid butyl ester and 8-chloro-1-phenyl-3H-2-benzazepine-5-carboxylic acid butyl ester and 6.5 g (62.4 mmol) of formamidine acetate in 70 mL of ethanol. When the addition was complete stirring at room temperature was continued for 30 min. The reaction was diluted with water and extracted with methylene chloride. The methylene chloride solution was washed with water, dried over anhydrous sodium sulfate and concentrated at reduced pressure. The residue was crystallized from a mixture of ether and petroleum ether to give a yellow solid. Recrystallization from a mixture of ether and methylene chloride gave pale yellow prisms, mp 150°-155°.

後処理

  1. additionWhen the addition
  2. extractionextracted with methylene chloride
  3. washThe methylene chloride solution was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated at reduced pressure
  6. customThe residue was crystallized from a mixture of ether and petroleum ether
  7. customto give a yellow solid
  8. customRecrystallization
  9. additionfrom a mixture of ether and methylene chloride
  10. customgave pale yellow prisms, mp 150°-155°

出典と根拠

ORDレコード
ord-140f7313b6ef42dc95034580338763a9
出典データセット
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04548750

反応ノート

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