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Triethylamine → 4-[4-(2-tert-Butylphenyl)piperazin-1-yl]-N-[(cyclopropylmethyl)sulfamoyl]-4-oxobutanamide

HRID 534875
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인쇄 미리보기

반응식

HRID 534875 반응식
[C:1]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:11]1[CH2:16][CH2:15][N:14]([C:17](=[O:23])[CH2:18][CH2:19][C:20]([OH:22])=O)[CH2:13][CH2:12]1)([CH3:4])([CH3:3])[CH3:2].[CH:24]1([CH2:27][NH:28][S:29]([NH2:32])(=[O:31])=[O:30])[CH2:26][CH2:25]1.CC1C=CC=C([N+]([O-])=O)C=1C(OC(=O)C1C([N+]([O-])=O)=CC=CC=1C)=O.C(N(CC)CC)C>O.C(#N)C>[C:1]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N:11]1[CH2:16][CH2:15][N:14]([C:17](=[O:23])[CH2:18][CH2:19][C:20]([NH:32][S:29](=[O:31])(=[O:30])[NH:28][CH2:27][CH:24]2[CH2:26][CH2:25]2)=[O:22])[CH2:13][CH2:12]1)([CH3:3])([CH3:4])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 104726482-Methyl-6-nitrobenzoic anhydrideHCID 21041395N-(cyclopropylmethyl)sulfamideHCID 66750856HCID 66750856, 화합물

생성물 1

HCID 667927364-[4-(2-tert-Butylphenyl)piperazin-1-yl]-N-[(cyclopropylmethyl)sulfamoyl]-4-oxobutanamide수율 21%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6342Acetonitrile용매

실험 절차

A mixture of 4-[4-(2-tert-butylphenyl)piperazin-1-yl]-4-oxobutanoic acid obtained in Example 53 (500 mg), N-(cyclopropylmethyl)sulfamide (248 mg), 2-methyl-6-nitrobenzoic anhydride (692 mg), N,N-dimethylaminopyridine (192 mg), triethylamine (0.656 mL), and acetonitrile (10 mL) was stirred at room temperature for over-night. Water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to provide the title compound (148 mg, 21%) as a colorless solid.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-308fc3814ace4c45b19f40e6bdf8573d
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08853215B2

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