Dimethylformamide → HCID 13526425, 화합물

HRID 444290노트

반응식

HRID 444290 반응식
[C:1]([NH:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[N:12]=[C:13]([SH:26])[NH:14][C:15]=2[C:16]2[CH:21]=[CH:20][C:19]([NH:22][C:23](=[O:25])[CH3:24])=[CH:18][CH:17]=2)=[CH:7][CH:6]=1)(=[O:3])[CH3:2].Cl[CH2:28][CH2:29]Br.CN(C)C=O.C(=O)([O-])[O-].[K+].[K+]>O>[C:1]([NH:4][C:5]1[CH:6]=[CH:7][C:8]([C:11]2[N:12]3[C:13]([S:26][CH2:28][CH2:29]3)=[N:14][C:15]=2[C:16]2[CH:21]=[CH:20][C:19]([NH:22][C:23](=[O:25])[CH3:24])=[CH:18][CH:17]=2)=[CH:9][CH:10]=1)(=[O:3])[CH3:2]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 78491-Bromo-2-ChloroethaneHCID 11430Potassium CarbonateHCID 178474105HCID 178474105, 화합물

생성물 1

HCID 13526425HCID 13526425, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 10.0 g. (0.027 mole) of 4,5-bis-(p-acetamidophenyl)-2-mercaptoimidazole and 4.9 g. (0.034 mole) of 2-chloroethyl bromide in 80 ml. of sieve dried dimethylformamide was refluxed with stirring under nitrogen for 75 minutes. Potassium carbonate (3.8 g., 0.027 mole) was added and the suspension was refluxed for 2 hours, then allowed to cool to room temperature and poured into 650 ml. of water. The gum which formed was filtered off and crystallized from 50 ml. of hot methanol. The crystals were washed with cold methanol and ether and air dried to give 5,6-bis(p-acetamidophenyl)-2,3-dihydroimidazo[2,1-b]thiazole, m.p. 285°-290° C.

후처리

  1. additionA mixture of 10.0 g
  2. temperaturethe suspension was refluxed for 2 hours
  3. additionpoured into 650 ml
  4. customThe gum which formed
  5. filtrationwas filtered off
  6. customcrystallized from 50 ml
  7. washThe crystals were washed with cold methanol and ether and air
  8. customdried

출처 및 근거

ORD 기록
ord-e57405c2047f4ab3ad461e52a34bc4cf
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04263311

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