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Dimethylamine → HCID 20033708, 화합물

HRID 231681
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HRID 231681 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 6

HCID 674DimethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 20033691HCID 20033691, 화합물HCID 20033697HCID 20033697, 화합물HCID 20033730HCID 20033730, 화합물HCID 20033735HCID 20033735, 화합물

생성물 1

HCID 20033708
HCID 20033708, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b175ae911c3b44c9a9aa819c313750a0
출처 데이터셋
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04847289

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