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1,2-Dichloroethane → HCID 86679523, 화합물

HRID 1776567
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HRID 1776567 반응식
[C:1]([S:4][C:5]([CH3:19])([CH3:18])[CH:6]([NH:10][C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[C:7]([OH:9])=[O:8])(=[O:3])[CH3:2].C(Cl)CCl.[Cl:24][C:25]1[CH:26]=[N+:27]([O-:50])[CH:28]=[C:29]([Cl:49])[C:30]=1[CH2:31][C@@H:32]([C:34]1[CH:39]=[CH:38][C:37]([O:40][CH:41]([F:43])[F:42])=[C:36]([O:44][CH2:45][CH:46]2[CH2:48][CH2:47]2)[CH:35]=1)O>C(Cl)Cl.CN(C1C=CN=CC=1)C>[C:1]([S:4][C:5]([CH3:19])([CH3:18])[CH:6]([NH:10][C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[C:7]([O:9][C@H:32]([C:34]1[CH:39]=[CH:38][C:37]([O:40][CH:41]([F:42])[F:43])=[C:36]([O:44][CH2:45][CH:46]2[CH2:47][CH2:48]2)[CH:35]=1)[CH2:31][C:30]1[C:29]([Cl:49])=[CH:28][N+:27]([O-:50])=[CH:26][C:25]=1[Cl:24])=[O:8])(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 111,2-DichloroethaneHCID 71092687(S)-3,5-dichloro-4-(2-(3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl)-2-hydroxyethyl)pyridine 1-oxideHCID 86679522HCID 86679522, 화합물

생성물 1

HCID 86679523HCID 86679523, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매
HCID 6344
Dichloromethane
용매
2회

실험 절차

3-(acetylthio)-2-(tert-butoxycarbonylamino)-3-methylbutanoic acid (693 mg, 2.38 mmol) was dissolved in DCM (10 ml). DMAP (73 mg, 0.59 mmol), EDC (342 mg, 1.79 mmol), and (S)-3,5-dichloro-4-(2-(3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl)-2-hydroxyethyl)pyridine 1-oxide (500 mg, 1.19 mmol) were added, and the mixture stirred for 4 hours at RT. The reaction mixture was diluted with DCM and washed with NaHCO3 sat. sol. (10 ml), HCl 1N, brine, dried over Na2SO4 and evaporated under vacuum to give 1.06 g. Crude compound was used in the next step without further purification.

후처리

  1. washwashed with NaHCO3 sat. sol. (10 ml), HCl 1N, brine
  2. dry with materialdried over Na2SO4
  3. customevaporated under vacuum
  4. customto give 1.06 g
  5. customCrude compound was used in the next step without further purification

출처 및 근거

ORD 기록
ord-aa41d035705c43489f8e52f6090d4ff1
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09265768B2

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