Stannous chloride dihydrate → HCID 59625705, 화합물

HRID 409929노트

반응식

HRID 409929 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[CH:18]=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:11][C:10]=2[N+:19]([O-])=O)=[CH:4][CH:3]=1.O.O.Cl[Sn]Cl.C([O-])(O)=O.[Na+]>CCO>[NH2:19][C:10]1[CH:11]=[C:12]([CH:17]=[CH:18][C:9]=1[NH:8][C:5]1[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=1)[C:13]([O:15][CH3:16])=[O:14]

참가 물질

5

반응물 3

HCID 61436Stannous chloride dihydrateHCID 516892Sodium BicarbonateHCID 59625834HCID 59625834, 화합물

생성물 1

HCID 59625705HCID 59625705, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
80 °C

실험 절차

A mixture of 27c (1.4 g, 4.8 mmol) and SnCl2.2H2O (4.9 g, 21.7 mmol) in EtOH (50 mL) was stirred at 80° C. After 4 h, the mixture was cooled to room temperature and was slowly added to saturated aqueous NaHCO3. The solid was filtered and washed with H2O. The solid was triturated with EtOAc and the filtrate was concentrated. The crude product 27d was used in the next reaction without purification. MS m/z (M+H+) 261.1.

후처리

  1. temperaturethe mixture was cooled to room temperature
  2. filtrationThe solid was filtered
  3. washwashed with H2O
  4. customThe solid was triturated with EtOAc
  5. concentrationthe filtrate was concentrated
  6. customThe crude product 27d was used in the next reaction without purification

출처 및 근거

ORD 기록
ord-e010f44bec014e43803a1e91883bbfbf
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08759533B2

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