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

HRID 534875
ノート
印刷プレビュー

反応式

HRID 534875 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 104726482-Methyl-6-nitrobenzoic anhydrideHCID 21041395N-(cyclopropylmethyl)sulfamideHCID 66750856HCID 66750856、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-308fc3814ace4c45b19f40e6bdf8573d
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08853215B2

反応ノート

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