(NE)-N-(3-chloro-4-oxonaphthalen-1-ylidene)thiophene-2-sulfonamide → N-(3-(1-methyl-1H-tetrazol-5-ylthio)-4-oxonaphthalen-1(4H)-ylidene)thiophene-2-sulfonamide

HRID 1258386

反応式

HRID 1258386 の反応式
Cl[C:2]1[C:11](=[O:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)/[C:4](=[N:13]/[S:14]([C:17]2[S:18][CH:19]=[CH:20][CH:21]=2)(=[O:16])=[O:15])/[CH:3]=1.[CH3:22][N:23]1[C:27]([SH:28])=[N:26][N:25]=[N:24]1>C1COCC1>[CH3:22][N:23]1[C:27]([S:28][C:2]2[C:11](=[O:12])[C:10]3[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=3)[C:4](=[N:13][S:14]([C:17]3[S:18][CH:19]=[CH:20][CH:21]=3)(=[O:16])=[O:15])[CH:3]=2)=[N:26][N:25]=[N:24]1

参加物

4

反応物 2

HCID 22524852(NE)-N-(3-chloro-4-oxonaphthalen-1-ylidene)thiophene-2-sulfonamideHCID 178482017HCID 178482017、化合物

生成物 1

HCID 67329899N-(3-(1-methyl-1H-tetrazol-5-ylthio)-4-oxonaphthalen-1(4H)-ylidene)thiophene-2-sulfonamide収率 68.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

36 mg (E)-N-(3-chloro-4-oxonaphthalen-1(4H)-ylidene)-thiophene-2-sulfonamide (12a) was dissolved in 3 ml THF, to which was added 11.7 mg 1-methyl-tetrazole-5-thiol. The reaction mixture was stirred at r.t. for 2 hrs and concentrated via rotavap. The residue was dissolved in dichloromethylene and triturated with hexane. The precipitate was filtered and washed with dichloromethylene/hexane (1:1) affording the title compound 28.8 mg (68.9%) as an orange-red solid, m.p.: 172° C. (dec.).

後処理

  1. concentrationconcentrated via rotavap
  2. dissolutionThe residue was dissolved in dichloromethylene
  3. customtriturated with hexane
  4. filtrationThe precipitate was filtered
  5. washwashed with dichloromethylene/hexane (1:1)

出典と根拠

ORDレコード
ord-242186a6e13440ddb39f07699d0a0194
出典データセット
uspto-grants-2013_06
特許番号
US08466157B2

関連ノート

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