Methane → HCID 131712839, 화합물

HRID 1702847

반응식

HRID 1702847 반응식
[CH2:1]([O:3][C:4]([C:6]1[C:7]([Cl:16])=[N:8][C:9]2[C:14]([N:15]=1)=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:5])[CH3:2].C.[CH2:18]([NH:22][C:23]([NH:25][CH2:26][CH2:27][CH2:28][CH3:29])=[S:24])[CH2:19][CH2:20][CH3:21]>CC(C)=O>[ClH:16].[CH2:1]([O:3][C:4]([C:6]1[C:7]([S:24][C:23]([NH:25][CH2:26][CH2:27][CH2:28][CH3:29])=[N:22][CH2:18][CH2:19][CH2:20][CH3:21])=[N:8][C:9]2[C:14]([N:15]=1)=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:5])[CH3:2]

참가 물질

5

반응물 3

HCID 297Methane2회HCID 2723622N,N'-DibutylthioureaHCID 12283436Ethyl 3-Chloroquinoxaline-2-carboxylate

생성물 1

HCID 131712839HCID 131712839, 화합물수율 47.5%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

2-Chloro-3-quinoxalinecarboxylic acid ethyl ester (7.10 g., 0.03 mole) was dissolved in 125 ml. of acetone treated with Norit and filtered. The filtrate was added to 5.650 g. (0.03 mole) of 1,3-di-n-butylthiourea in 100 ml. of acetone. The solution was stirred at reflux under a nitrogen atmosphere for 6 hours, allowed to cool to room temperature, and stirred an additional 17 hours. The red solution was treated with Norit, filtered, and concentrated to a volume of 100 ml. The yellow solid that crystallized out was collected by filtration, washed and dried to give the 6.05 g. (47.5% yield) of product, m.p. 138°-139° C. (dec.).

후처리

  1. filtrationfiltered
  2. additionThe filtrate was added to 5.650 g
  3. temperatureat reflux under a nitrogen atmosphere for 6 hours
  4. stirringstirred an additional 17 hours
  5. filtrationfiltered
  6. concentrationconcentrated to a volume of 100 ml
  7. customThe yellow solid that crystallized out
  8. filtrationwas collected by filtration
  9. washwashed
  10. customdried
  11. customto give the 6.05 g

출처 및 근거

ORD 기록
ord-f825206e528846759b677540039b12f1
출처 데이터셋
uspto-grants-1982_09
특허 번호
US04349674

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