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4-Methoxybenzenesulfonyl chloride → HCID 69310689, 화합물

HRID 751469
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HRID 751469 반응식
[C:1]([O:5][C:6](=[O:24])[NH:7][C@H:8]([C:13](=[O:23])[NH:14][CH:15]1[CH2:21][CH2:20][CH2:19][NH:18][CH2:17][CH:16]1[OH:22])[CH2:9][CH:10]([CH3:12])[CH3:11])([CH3:4])([CH3:3])[CH3:2].[CH3:25][O:26][C:27]1[CH:32]=[CH:31][C:30]([S:33](Cl)(=[O:35])=[O:34])=[CH:29][CH:28]=1>ClCCCl>[C:1]([O:5][C:6](=[O:24])[NH:7][C@H:8]([C:13](=[O:23])[NH:14][CH:15]1[CH2:21][CH2:20][CH2:19][N:18]([S:33]([C:30]2[CH:29]=[CH:28][C:27]([O:26][CH3:25])=[CH:32][CH:31]=2)(=[O:35])=[O:34])[CH2:17][CH:16]1[OH:22])[CH2:9][CH:10]([CH3:12])[CH3:11])([CH3:3])([CH3:4])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 74014-Methoxybenzenesulfonyl chlorideHCID 12076054HCID 12076054, 화합물2회

생성물 1

HCID 69310689HCID 69310689, 화합물

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매2회

실험 절차

[(S)-1-(3-Hydroxy-azepan-4-ylcarbamoyl)-3-methyl-butyl]-carbamic acid-tert-butyl ester (compound 2g, 0.8 g, 2.33 mmol) was dissolved in 1,2-dichloroethane (DCE, 20 ml). Then, morpholinemethyl polystyrene resin beads (1.26 g, 3.7 mmol/g, Nova) were added and the solution was shaken for 5 minutes. Then, p-methoxybenzenesulfonyl chloride (0.48 g, 2.33 mmol) was dissolved in DCE (10 ml), and this solution was added to the reaction mixture. The reaction was shaken overnight, filtered, washed with DCE (2×10 ml), then CH2Cl2 (10 ml). The combined organics were concentrated in vacuo, and used in the next reaction without further purification: M+H+=514.2.

후처리

  1. additionwere added
  2. additionthis solution was added to the reaction mixture
  3. stirringThe reaction was shaken overnight
  4. filtrationfiltered
  5. washwashed with DCE (2×10 ml)
  6. concentrationThe combined organics were concentrated in vacuo
  7. customused in the next reaction without further purification

출처 및 근거

ORD 기록
ord-c369d8bcc5014b5d9cbe3305d4679179
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07405209B2

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