Methane → HCID 70523752, 화합물

HRID 904857노트

반응식

HRID 904857 반응식
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

참가 물질

5

반응물 3

HCID 297MethaneHCID 132351-Adamantanecarboxylic acidHCID 20477848HCID 20477848, 화합물

생성물 1

HCID 70523752HCID 70523752, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-e38e4850413848bebccf3521ef066ab7
출처 데이터셋
uspto-grants-1983_12
특허 번호
US04420487

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