Methane → HCID 70523752、化合物

HRID 904857ノート

反応式

HRID 904857 の反応式
Cl.Cl.[NH2:3][C:4]1[CH:10]=[C:9]([Cl:11])[C:8]([S:12](=[O:15])(=[O:14])[NH2:13])=[CH:7][C:5]=1[NH2:6].[C:16]12(C(O)=O)[CH2:25][CH:20]3[CH2:21][CH:22]([CH2:24][CH:18]([CH2:19]3)[CH2:17]1)[CH2:23]2.[CH4:29]>CO>[OH2:14].[CH:16]12[CH2:17][CH:18]3[CH2:19][CH:20]([CH2:21][CH:22]([CH2:24]3)[CH:23]1[C:29]1[NH:6][C:5]3[CH:7]=[C:8]([S:12](=[O:14])(=[O:15])[NH2:13])[C:9]([Cl:11])=[CH:10][C:4]=3[N:3]=1)[CH2:25]2.[CH:16]12[CH2:17][CH:18]3[CH2:19][CH:20]([CH2:21][CH:22]([CH2:24]3)[CH:23]1[C:29]1[NH:6][C:5]3[CH:7]=[C:8]([S:12](=[O:14])(=[O:15])[NH2:13])[C:9]([Cl:11])=[CH:10][C:4]=3[N:3]=1)[CH2:25]2

参加物

5

反応物 3

HCID 297MethaneHCID 132351-Adamantanecarboxylic acidHCID 20477848HCID 20477848、化合物

生成物 1

HCID 70523752HCID 70523752、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A mixture of 2.95 g of 2-amino-4-chloro-5-sulfamylaniline dihydrochloride and 2.70 g of 1-adamantanecarboxylic acid was ground together and heated at 190°-200° for 5 hours. The dark solid was dissolved in 500 ml of methanol, the methanol brought to a boil, charcoal added, boiling continued for five minutes, and the suspension then filtered through two sheets of filter paper, and then through Celite. Concentration in vacuo provided a solid which was then added to 100 ml of concentrated ammonium hydrozide and stirred for twenty minutes. The crude product was collected by filtration and recrystallized from acetonitrile to provide 0.5 g of colorless crystals, m.p. 207°-210°.

後処理

  1. temperatureheated at 190°-200° for 5 hours
  2. additionadded
  3. filtrationthe suspension then filtered through two sheets of filter paper
  4. concentrationConcentration in vacuo
  5. customprovided a solid which
  6. filtrationThe crude product was collected by filtration
  7. customrecrystallized from acetonitrile

出典と根拠

ORDレコード
ord-e38e4850413848bebccf3521ef066ab7
出典データセット
uspto-grants-1983_12
特許番号
US04420487

反応ノート

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