1,8-Diazabicyclo(5.4.0)undec-7-ene → N-ethyl-N'-[7-(phenylsulfanyl)-4,5-dihydro-1,3-benzothiazol-2-yl]urea

HRID 9159노트

반응식

HRID 9159 반응식
[C:1]1([S:7][C:8]2(SC3C=CC=CC=3)[C:16]3[S:15][C:14]([NH:17][C:18]([NH:20][CH2:21][CH3:22])=[O:19])=[N:13][C:12]=3[CH2:11][CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1CCN2C(=NCCC2)CC1>C1COCC1>[CH2:21]([NH:20][C:18]([NH:17][C:14]1[S:15][C:16]2[C:8]([S:7][C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)=[CH:9][CH2:10][CH2:11][C:12]=2[N:13]=1)=[O:19])[CH3:22]

참가 물질

4

반응물 2

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 21985555N-[7,7-Di(phenylsulfanyl)-4,5,6,7-tetrahydro-1,3-benzothiazol-2-yl]-N'-ethylurea

생성물 1

HCID 21985581N-ethyl-N'-[7-(phenylsulfanyl)-4,5-dihydro-1,3-benzothiazol-2-yl]urea

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
20 °C

실험 절차

To a suspension of N-[7,7-di(phenylsulfanyl)-4,5,6,7-tetrahydro-1,3-benzothiazol-2-yl]-N′-ethylurea (700 mg, 1.59 mmol) in THF (14.0 mL) was added DBU (0.36 mL, 2.38 mmol). The reaction mixture was stirred at about 20° C. for about 30 min. The reaction was concentrated in vacuo. The residual yellow oil was taken up in CH2Cl2, washed with AcOH/H2O 1/10 and dried over MgSO4. The organic solvent was removed in vacuo and the residual oil (1.0 g) was used in the next step without further purification.

후처리

  1. concentrationThe reaction was concentrated in vacuo
  2. washwashed with AcOH/H2O 1/10
  3. dry with materialdried over MgSO4
  4. customThe organic solvent was removed in vacuo
  5. customthe residual oil (1.0 g) was used in the next step without further purification

출처 및 근거

ORD 기록
ord-f52c1f5594b74389a752e81d2ba57891
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091227B2

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