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Hydrochloric Acid → N-({6-[(2-Hydroxyethyl)amino]-4-(methylthio)pyridin-2-yl}carbamoyl)-5-(2-methoxyethyl)-4-methylthiophene-2-sulfonamide

HRID 1696750
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HRID 1696750 반응식
C([Si](C)(C)[O:6][CH2:7][CH2:8][NH:9][C:10]1[N:15]=[C:14]([NH:16][C:17]([NH:19][S:20]([C:23]2[S:24][C:25]([CH2:29][CH2:30][O:31][CH3:32])=[C:26]([CH3:28])[CH:27]=2)(=[O:22])=[O:21])=[O:18])[CH:13]=[C:12]([S:33][CH3:34])[CH:11]=1)(C)(C)C.Cl>CO>[OH:6][CH2:7][CH2:8][NH:9][C:10]1[N:15]=[C:14]([NH:16][C:17]([NH:19][S:20]([C:23]2[S:24][C:25]([CH2:29][CH2:30][O:31][CH3:32])=[C:26]([CH3:28])[CH:27]=2)(=[O:22])=[O:21])=[O:18])[CH:13]=[C:12]([S:33][CH3:34])[CH:11]=1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 67273738HCID 67273738, 화합물

생성물 1

HCID 42629875N-({6-[(2-Hydroxyethyl)amino]-4-(methylthio)pyridin-2-yl}carbamoyl)-5-(2-methoxyethyl)-4-methylthiophene-2-sulfonamide수율 63.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The below prepared N-({6-[(2-(tert-butyl-dimethyl-silanyloxy)-ethyl)amino]-4-(methylthio)pyridin-2-yl}carbamoyl)-5-(2-methoxyethyl)-4-methylthiophene-2-sulfonamide (0.160 g, 0.278 mmol) was dissolved in 5 mL of MeOH and treated with aq. HCl (1.0 mL 1 N). After 2 h at ambient temperature, the reaction mixture was poured onto icewater, twofold extracted with AcOEt, washed with water and brine, dried over magnesium sulfate, and evaporated to dryness. Crystallization from AcOEt gave 0.081 g of the title compound as off-white crystals.

후처리

  1. additionthe reaction mixture was poured onto icewater
  2. extractiontwofold extracted with AcOEt
  3. washwashed with water and brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated to dryness
  6. customCrystallization from AcOEt

출처 및 근거

ORD 기록
ord-b0fe534236334865b34784227f8c8609
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08163778B2

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