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Dimethylamine → HCID 20033708、化合物

HRID 231681
ノート
印刷プレビュー

反応式

HRID 231681 の反応式
[C:1]([CH2:4][C:5]1[CH:10]=[CH:9][C:8]([S:11]([C:14]2[S:18][C:17]([S:19]([NH2:22])(=[O:21])=[O:20])=[CH:16][CH:15]=2)(=[O:13])=[O:12])=[CH:7][CH:6]=1)(O)=[O:2].[C:23](N1C=CN=C1)([N:25]1C=CN=[CH:26]1)=O.CNC.C(NC(CC1C=CC(S(C2SC(S(N)(=O)=O)=CC=2)(=O)=O)=CC=1)=O)C.CNC(CCC1C=CC(S(C2SC(S(N)(=O)=O)=CC=2)(=O)=O)=CC=1)=O.CN(C)C(CCCC1C=CC(S(C2SC(S(N)(=O)=O)=CC=2)(=O)=O)=CC=1)=O>O1CCCC1>[CH3:23][N:25]([CH3:26])[C:1]([CH2:4][C:5]1[CH:10]=[CH:9][C:8]([S:11]([C:14]2[S:18][C:17]([S:19]([NH2:22])(=[O:21])=[O:20])=[CH:16][CH:15]=2)(=[O:13])=[O:12])=[CH:7][CH:6]=1)=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 674DimethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 20033691HCID 20033691、化合物HCID 20033697HCID 20033697、化合物HCID 20033730HCID 20033730、化合物HCID 20033735HCID 20033735、化合物

生成物 1

HCID 20033708
HCID 20033708、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

5-(4-carboxymethylphenylsulfonyl)thiophene-2-sulfonamide (1.6 g) was dissolved in 50 ml of tetrahydrofuran and 0.72 g of carbonyldiimidazole was added. After stirring for one hour at room temperature excess aqueous dimethylamine was added and the mixture stirred overnight. The reaction mixture was concentrated under vacuum and the residue partitioned between ethyl acetate and water. The organic phase was separated, dried over sodium sulfate and concentrated under vacuum, giving an oil weighing 1.35 g, N.M.R. (acetone, d6) δ: 2.92 (3H, s), 3.08 (3H, s), 3.84 (2H, s), 7.02 (2H, s), 7.50 (3H, m), 7.65 (1H, d), 7.90 (2H, d). The following compounds were also made by similar procedures: 5-(4-ethylcarbamoylmethylphenylsulfonyl)thiophene-2-sulfonamide, 5-[4-(2-methylcarbamoylethyl)phenylsulfonyl]thiophene-2-sulfonamide, and 5-[4-(3-dimethylcarbamoylpropyl)phenylsulfonyl]thiophene-2-sulfonamide.

後処理

  1. additionwas added
  2. concentrationThe reaction mixture was concentrated under vacuum
  3. customthe residue partitioned between ethyl acetate and water
  4. customThe organic phase was separated
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under vacuum
  7. customgiving an oil

出典と根拠

ORDレコード
ord-b175ae911c3b44c9a9aa819c313750a0
出典データセット
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04847289

反応ノート

読み込み中…

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