Water → HCID 10954430, 화합물

HRID 989323노트

반응식

HRID 989323 반응식
[NH2:1][C:2]1[C:3]2[CH:14]=[C:13]([N+:15]([O-:17])=[O:16])[CH:12]=[CH:11][C:4]=2[S:5][C:6]=1C(OC)=O.O>CN1CCCC1=O.CN1CCNCC1>[NH2:1][C:2]1[C:3]2[CH:14]=[C:13]([N+:15]([O-:17])=[O:16])[CH:12]=[CH:11][C:4]=2[S:5][CH:6]=1

참가 물질

5

반응물 2

HCID 962WaterHCID 2759774methyl 3-amino-5-nitro-1-benzothiophene-2-carboxylate

생성물 1

HCID 10954430HCID 10954430, 화합물

시약·촉매·용매 2

HCID 13387N-methyl-2-pyrrolidone용매HCID 531671-Methylpiperazine용매

실험 절차

A solution of 23.00 g (91.26 mmol) of methyl 3-amino-5-nitrobenzo[b]thiophene-2-carboxylate (J. Hetero. Chem., 34(4), 1163 (1997)) in 100 mL of 1-methyl-2-pyrrolidinone and 30 mL of 1-methylpiperazine is heated at 180° C. for 2 hours. The reaction is cooled to room temperature and poured into water. The resultant solid is collected by filtration and washed with water. The solid is dissolved in a mixture of ethyl acetate and diethyl ether and the solution is washed with water twice. The organic layer is dried over magnesium sulfate, filtered and concentrated in vacuo. Diethyl ether and hexane are added to the residue and the dark red solid is collected by filtration to provide 11.17 g (63%), mp 155-158° C.

후처리

  1. filtrationThe resultant solid is collected by filtration
  2. washwashed with water
  3. dissolutionThe solid is dissolved in a mixture of ethyl acetate and diethyl ether
  4. washthe solution is washed with water twice
  5. dry with materialThe organic layer is dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. additionDiethyl ether and hexane are added to the residue
  9. filtrationthe dark red solid is collected by filtration
  10. customto provide 11.17 g (63%), mp 155-158° C.

출처 및 근거

ORD 기록
ord-75bdc5281afb4cb49132c96f25f7e1ae
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06638929B2

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