Triethylamine → HCID 57773557、化合物

HRID 333115

反応式

HRID 333115 の反応式
[N:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10]([NH2:13])(=[O:12])=[O:11])=[CH:6][CH:5]=1)=[C:2]=[S:3].C(N(CC)CC)C.Cl.[I:22][C:23]1[CH:24]=[C:25]([CH:28]=[CH:29][CH:30]=1)[CH2:26][NH2:27]>C(#N)C>[I:22][C:23]1[CH:24]=[C:25]([CH:28]=[CH:29][CH:30]=1)[CH2:26][NH:27][C:2](=[S:3])[NH:1][C:4]1[CH:5]=[CH:6][C:7]([S:10]([NH2:13])(=[O:11])=[O:12])=[CH:8][CH:9]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 5213594-IsothiocyanatobenzenesulfonamideHCID 27238613-Iodobenzylamine hydrochloride

生成物 1

HCID 57773557HCID 57773557、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a suspension of 4-isothiocyanatobenzenesulfonamide (378 mg, 1.76 mmol) in dry acetonitrile (10 mL) and triethylamine (0.3 mL, 4.0 mmol) was added 3-iodobenzylamine hydrochloride salt (476 mg, 1.76 mmol). The reaction mixture became warm and a clear solution resulted. After stirring for 2 h the reaction was concentrated and the crude solid recrystallized from methanol/water to afford a white solid. The solid was filtered and washed with hexanes to afford the desired product MIP-1139 (715 mg, 91%). 1H NMR (400 MHz, DMSO-d6) δ 9.95 (br, 1H), 8.48 (br, 1H), 7.74-7.61 (m, 5H), 7.36-7.12 (m, 3H), 4.70 (m, 2H); (M+H)+ (448).

後処理

  1. temperatureThe reaction mixture became warm
  2. customa clear solution resulted
  3. concentrationwas concentrated
  4. customthe crude solid recrystallized from methanol/water
  5. customto afford a white solid
  6. filtrationThe solid was filtered
  7. washwashed with hexanes

出典と根拠

ORDレコード
ord-bed49e7bedfa453d8f95e0393c47a205
出典データセット
uspto-grants-2014_11
特許番号
US08877970B2

関連ノート

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