2-Chloroadenosine → 2-Hydrazinoadenosine

HRID 2242475

반응식

HRID 2242475 반응식
O.[NH2:2][NH2:3].Cl[C:5]1[N:6]=[C:7]([NH2:23])[C:8]2[N:9]=[CH:10][N:11]([C:21]=2[N:22]=1)[C@@H:12]1[O:20][C@H:17]([CH2:18][OH:19])[C@@H:15]([OH:16])[C@H:13]1[OH:14]>O>[NH:2]([C:5]1[N:6]=[C:7]([NH2:23])[C:8]2[N:9]=[CH:10][N:11]([C:21]=2[N:22]=1)[C@@H:12]1[O:20][C@H:17]([CH2:18][OH:19])[C@@H:15]([OH:16])[C@H:13]1[OH:14])[NH2:3]

참가 물질

4

반응물 2

HCID 89742-Chloroadenosine2회HCID 24654Hydrazine hydrate (1:1)

생성물 1

HCID 103572622-Hydrazinoadenosine

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
62 °C

실험 절차

A reaction vessel is charged with hydrazine hydrate (1285 g). The solution is heated to approximately 62° C., and 2-chloroadenosine (500 g) is added while maintaining the temperature of approximately 62° C. The mixture is maintained at a target of 62° C. for at least 2 hours, until the level of residual 2-chloroadenosine in the mixture is not more than 0.10%. The mixture is cooled to approximately 40° C. and the mixture is checked to verify the presence of solids. Water (2275 g) is slowly added while maintaining the temperature at approximately 40° C. The mixture is cooled to approximately 10° C. and held for not less than 1 hour. The product is isolated by filtration, washed with water (1195 g) and then with absolute ethanol (1885 g). The product is dried under vacuum at up to 30° C. for not less than 12 hours, to give 2-hydrazinoadenosine.

후처리

  1. temperaturewhile maintaining the temperature of approximately 62° C
  2. temperatureThe mixture is cooled to approximately 40° C.
  3. temperaturewhile maintaining the temperature at approximately 40° C
  4. temperatureThe mixture is cooled to approximately 10° C.
  5. waitheld for not less than 1 hour
  6. customThe product is isolated by filtration
  7. washwashed with water (1195 g)
  8. customThe product is dried under vacuum at up to 30° C. for not less than 12 hours

출처 및 근거

ORD 기록
ord-1283df27c5914139befea77a4039171e
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07671192B2

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