Dimethylformamide → HCID 13526425、化合物

HRID 444290ノート

反応式

HRID 444290 の反応式
[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]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 78491-Bromo-2-ChloroethaneHCID 11430Potassium CarbonateHCID 178474105HCID 178474105、化合物

生成物 1

HCID 13526425HCID 13526425、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e57405c2047f4ab3ad461e52a34bc4cf
出典データセット
uspto-grants-1981_04
特許番号
US04263311

反応ノート

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