Hydrochloric Acid → HCID 22873065, 화합물

HRID 1781573노트

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HRID 1781573 반응식
[Br:1][C@@H:2]1[C@:6](C(=O)C)([OH:7])[C@@H:5]([CH2:11][O:12][C:13](=[O:15])[CH3:14])[O:4][C@H:3]1[N:16]1[CH:23]=[C:22]([CH3:24])[C:20](=[O:21])[NH:19][C:17]1=[O:18].O.NN.Cl>O.C(#N)C>[Br:1][C@@H:2]1[C@H:6]([OH:7])[C@@H:5]([CH2:11][O:12][C:13](=[O:15])[CH3:14])[O:4][C@H:3]1[N:16]1[CH:23]=[C:22]([CH3:24])[C:20](=[O:21])[NH:19][C:17]1=[O:18]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 24654Hydrazine hydrate (1:1)HCID 67581565HCID 67581565, 화합물

생성물 1

HCID 22873065HCID 22873065, 화합물수율 92.9%

시약·촉매·용매 2

HCID 962Water용매2회HCID 6342Acetonitrile용매

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온도
0 °C

실험 절차

400 ml of acetonitrile and 2.16 g (3 equivalents) of water were added to 16.2 g (40.0 mmol) of 2'-deoxy-2'-bromo-3',5'-O-diacetyl-5-methyluridine, and the mixture was stirred. The resulting solution was cooled to 0° C., 6.01 g (3 equivalents) of hydrazine monohydrate were added thereto, and the mixture was reacted for 20 hours at that temperature. 100 ml of water were added to the reaction mixture, which was then neutralized to a pH of 6.8 by adding 6 N-hydrochloric acid thereto. The acetonitrile layer was separated, washed with saturated saline solution, dried with anhydrous magnesium sulfate, and then concentrated under reduced pressure to obtain 13.5 g of 2'-deoxy-2'-bromo-5'-O-acetyl-5-methyluridine. Its purity was 81.8%. Its yield was 76.0%.

후처리

  1. customthe mixture was reacted for 20 hours at that temperature
  2. customThe acetonitrile layer was separated
  3. washwashed with saturated saline solution
  4. dry with materialdried with anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-1599ec65fdd54d67a7b447137a9c1a30
출처 데이터셋
uspto-grants-1997_05
특허 번호
US05633366

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