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Hydrazine, dihydrochloride → HCID 178521699, 화합물

HRID 1040442
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HRID 1040442 반응식
[CH2:1]([O:8][C:9](=[O:21])[NH:10][C:11]1([C:14](=O)/[N:15]=[CH:16]/[N:17](C)C)[CH2:13][CH2:12]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.Cl.[NH2:24]N.CCOC(C)=O.O>CC(O)=O>[CH2:1]([O:8][C:9](=[O:21])[NH:10][C:11]1([C:14]2[NH:15][CH:16]=[N:17][N:24]=2)[CH2:13][CH2:12]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 17548Hydrazine, dihydrochlorideHCID 22728543Water ethylacetateHCID 178484344HCID 178484344, 화합물

생성물 1

HCID 178521699HCID 178521699, 화합물수율 68.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
90 °C

실험 절차

To a solution of (1-{[1-dimethylamino-meth-(E)-ylidene]-carbamoyl}-cyclopropyl)-carbamic acid benzyl ester (1.11 g, 3.83 mmol) in AcOH (6 ml) was added hydrazine dihydrochloride (803 mg, 7.65 mmol). The reaction mixture was stirred at 90° C. for 1.5 h. The reaction mixture was poured into EtOAc/water. The organic phase was separated, washed with water, sat. NaHCO3, brine, dried over anhydrous Na2SO4, filtered, concentrated and dried under high vacuum to afford 677 mg of [1-(4H-[1,2,4]triazol-3-yl)-cyclopropyl]-carbamic acid benzyl ester as a off-white solid, m/z 259.6 [M+1]+.

후처리

  1. customThe organic phase was separated
  2. washwashed with water, sat. NaHCO3, brine
  3. dry with materialdried over anhydrous Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customdried under high vacuum

출처 및 근거

ORD 기록
ord-1b7eafbeadd64fb99c81afe6bf06a9ac
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08552205B2

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