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Ammonium Bicarbonate → HCID 68697939, 화합물

HRID 1437384
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HRID 1437384 반응식
[C:1]([O:5][C:6]([NH:8][C@@H:9]1[CH2:14][CH2:13][C@@H:12]([C:15](O)=[O:16])[CH2:11][C@H:10]1[O:18][CH3:19])=[O:7])([CH3:4])([CH3:3])[CH3:2].O[N:21]1C2N=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC.C(=O)([O-])O.[NH4+]>CN(C=O)C>[C:1]([O:5][C:6](=[O:7])[NH:8][C@@H:9]1[CH2:14][CH2:13][C@@H:12]([C:15](=[O:16])[NH2:21])[CH2:11][C@H:10]1[O:18][CH3:19])([CH3:4])([CH3:3])[CH3:2]
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참가 물질

6

반응물 4

HCID 14013Ammonium BicarbonateHCID 181649HOAtHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 68700284HCID 68700284, 화합물

생성물 1

HCID 68697939HCID 68697939, 화합물수율 75.9%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

A solution of the acid (f) (5.0 g, 18 mmol) and 1-hydroxy-7-azabenzotriazole (2.73 g, 20 mmol) in DMF (200 ml) was treated with (3-dimethylamino-propyl)-ethyl-carbodiimide hydrochloride (3.87 g, 20 mmol) and ammonium hydrogen carbonate (5.8 g, 73 mmol). The mixture was stirred at room temperature for 18 hours then evaporated to dryness. The residue was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate solution. The organic extract was dried and evaporated. Trituration with ether and filtration afforded a white solid (3.72 g, 75%).

후처리

  1. customthen evaporated to dryness
  2. customThe residue was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate solution
  3. extractionThe organic extract
  4. customwas dried
  5. customevaporated
  6. filtrationTrituration with ether and filtration

출처 및 근거

ORD 기록
ord-992b3701e03f4cb9894b71198317554a
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07622481B2

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