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Dimethylformamide → HCID 57966935, 화합물

HRID 420585
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HRID 420585 반응식
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[N:6]=[C:7]([N:9]3[CH2:13][CH2:12][CH:11]([NH2:14])[CH2:10]3)[S:8][C:4]=2[CH:3]=1.[N+:17]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[S:26](Cl)(=[O:28])=[O:27])([O-:19])=[O:18].C(N(CC)CC)C.CN(C)C=O>O>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[N:6]=[C:7]([N:9]3[CH2:13][CH2:12][CH:11]([NH:14][S:26]([C:21]4[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=4[N+:17]([O-:19])=[O:18])(=[O:27])=[O:28])[CH2:10]3)[S:8][C:4]=2[CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 155402-Nitrobenzenesulfonyl chlorideHCID 579660771-(6-Chlorobenzothiazole-2-yl)pyrrolidine-3-ylamine

생성물 1

HCID 57966935HCID 57966935, 화합물수율 46.7%

시약·촉매·용매 1

HCID 962Water
용매

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온도
60 °C

실험 절차

A mixture of 1-(6-chlorobenzothiazole-2-yl)pyrrolidine-3-ylamine (2.49 g), 2-nitrobenzenesulphonyl chloride (2.40 g), triethylamine (3.02 mL) and dimethylformamide (15 mL) was stirred at 60° C. for 3 hours. To the reaction solution was added water and extracted with ethyl acetate. The organic layer was washed with water and brine, and dried over sodium sulphate. The solvent was evaporated under reduced pressure and the residue was purified by column chromatograph on silica gel to give the title compound (2.01 g). Yield: 47

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water and brine
  3. dry with materialdried over sodium sulphate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by column chromatograph on silica gel

출처 및 근거

ORD 기록
ord-03f0843a6d234d5c9e63d67b786d3d5b
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08097610B2

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