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Formic Acid → 2-((6,11-Dihydro-5H-dibenzo[b,e]azepin-6-yl)methyl)isoindoline-1,3-dione

HRID 1033849
ノート
印刷プレビュー

反応式

HRID 1033849 の反応式
[C:1]1(=[O:27])[N:5]([CH2:6][C:7]2[NH:13][C:12]3[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=3[CH:10]=[C:9]3[CH:18]=[CH:19][CH:20]=[CH:21][C:8]=23)[C:4](=[O:22])[C:3]2=[CH:23][CH:24]=[CH:25][CH:26]=[C:2]12.C(O)=O.[H][H]>CN(C)C=O.[Pd]>[C:4]1(=[O:22])[N:5]([CH2:6][CH:7]2[NH:13][C:12]3[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=3[CH2:10][C:9]3[CH:18]=[CH:19][CH:20]=[CH:21][C:8]2=3)[C:1](=[O:27])[C:2]2=[CH:26][CH:25]=[CH:24][CH:23]=[C:3]12
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 284Formic AcidHCID 190249922-(5H-Dibenz[B,E]azepin-6-ylmethyl)-1H-isoindole-1,3(2H)-dioneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 99466272-((6,11-Dihydro-5H-dibenzo[b,e]azepin-6-yl)methyl)isoindoline-1,3-dione

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 6228
Dimethylformamide
溶媒
2 回

反応条件

温度
50 °C

実験手順

A suspension of 110.0 kg of 6-phthalimidomethyl-5H-dibenz[b,e]azepine in 911.4 liters of dimethylformamide, 28.7 kg of formic acid and a suspension of 12.5 kg of 10% palladium charcoal in 25 liters of dimethylformamide is fed into a 1200 liter VA-propulsive jet loop reactor. The reaction mixture is heated to 70° C. and hydrogenated under 7 bar of absolute hydrogen pressure. After the catalyst has been filtered off and the reaction equipment and catalyst have been washed with 80 liters of dimethylformamide, 960 liters of dimethylformamide are distilled off from the combined filtrates at 70° to 80° C. After cooling to 50° C., 150 liters of acetone are added, then after further cooling to 15° C. the precipitated crystals are centrifuged off, washed with acetone and dried.

後処理

  1. customis fed into a 1200 liter VA-propulsive jet loop reactor
  2. filtrationAfter the catalyst has been filtered off
  3. washthe reaction equipment and catalyst have been washed with 80 liters of dimethylformamide, 960 liters of dimethylformamide
  4. distillationare distilled off from the combined filtrates at 70° to 80° C
  5. addition150 liters of acetone are added
  6. temperatureafter further cooling to 15° C. the precipitated crystals
  7. washwashed with acetone
  8. customdried

出典と根拠

ORDレコード
ord-7e6b63768c31432f833c6295e0411a32
出典データセット
uspto-grants-1994_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05312916

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート