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Triethylamine → Methanesulphonic Acid 1-{4-[1-(4-cyclohex-1-enyl-phenyl)-3-(3,5-dichlorophenyl)-ureidomethyl]phenyl}-2-(2H-tetrazol-5-yl)ethyl Ester

HRID 480384
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HRID 480384 반응식
[C:1]1([C:7]2[CH:12]=[CH:11][C:10]([N:13]([CH2:25][C:26]3[CH:31]=[CH:30][C:29]([CH:32]([OH:39])[CH2:33][C:34]4[N:35]=[N:36][NH:37][N:38]=4)=[CH:28][CH:27]=3)[C:14]([NH:16][C:17]3[CH:22]=[C:21]([Cl:23])[CH:20]=[C:19]([Cl:24])[CH:18]=3)=[O:15])=[CH:9][CH:8]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]=1.C(N(CC)CC)C.[CH3:47][S:48](Cl)(=[O:50])=[O:49].N12CCCN=C1CCCCC2>C(Cl)Cl>[C:1]1([C:7]2[CH:8]=[CH:9][C:10]([N:13]([CH2:25][C:26]3[CH:27]=[CH:28][C:29]([CH:32]([O:39][S:48]([CH3:47])(=[O:50])=[O:49])[CH2:33][C:34]4[N:35]=[N:36][NH:37][N:38]=4)=[CH:30][CH:31]=3)[C:14]([NH:16][C:17]3[CH:22]=[C:21]([Cl:23])[CH:20]=[C:19]([Cl:24])[CH:18]=3)=[O:15])=[CH:11][CH:12]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]=1
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HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 187689131-(4-Cyclohex-1-enylphenyl)-3-(3,5-dichlorophenyl)-1-{4-[1-hydroxy-2-(2H-tetrazol-5-yl)ethyl]benzyl}urea

생성물 1

HCID 20601515Methanesulphonic Acid 1-{4-[1-(4-cyclohex-1-enyl-phenyl)-3-(3,5-dichlorophenyl)-ureidomethyl]phenyl}-2-(2H-tetrazol-5-yl)ethyl Ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

1-(4-Cyclohex-1-enylphenyl)-3-(3,5-dichlorophenyl)-1-{4-[1-hydroxy-2-(2H-tetrazol-5-yl)ethyl]benzyl}urea (100 mg, 0.17 mmol) was dissolved in DCM (1 ml) and triethyl amine (27 μl, 0.195 mmol) was added. The mixture was cooled to 0° C. and methansulphonyl chloride (15 μl, 0.195 mmol) was added followed by 1,8-diazabicyclo[5,4,0]-undec-7-ene (29 μl, 0.195 mmol). The mixture was stirred at 0° C. for 2 hours, and at room temperature overnight, then diluted with DCM (20 ml) and washed with brine (20 ml). The organic solution was dried with anhydrous sodium sulphate and evaporated to dryness, to give pure title material as a white powder. Yield: 113 mg (100%).

후처리

  1. washwashed with brine (20 ml)
  2. dry with materialThe organic solution was dried with anhydrous sodium sulphate
  3. customevaporated to dryness
  4. customto give pure title material as a white powder

출처 및 근거

ORD 기록
ord-2c201c30739b448985d5226253ec6593
출처 데이터셋
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06649641B2

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