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Citric Acid → HCID 86710845, 화합물

HRID 1471803
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HRID 1471803 반응식
[CH3:1][N:2]([CH2:4]/[CH:5]=[CH:6]/[C:7]([NH:9][C:10]1[CH:11]=[C:12]2[C:25]([NH:26][C:27]3[CH:28]=[CH:29][C:30]([F:34])=[C:31]([Cl:33])[CH:32]=3)=[N:24][CH:23]=[N:22][C:13]2=[CH:14][C:15]=1[O:16][C@@H:17]1[CH2:21][O:20][CH2:19][CH2:18]1)=[O:8])[CH3:3].[C:35]([OH:47])(=[O:46])[CH2:36][C:37]([CH2:42][C:43]([OH:45])=[O:44])([C:39]([OH:41])=[O:40])[OH:38]>C(O)C>[CH3:1][N:2]([CH2:4]/[CH:5]=[CH:6]/[C:7]([NH:9][C:10]1[CH:11]=[C:12]2[C:25]([NH:26][C:27]3[CH:28]=[CH:29][C:30]([F:34])=[C:31]([Cl:33])[CH:32]=3)=[N:24][CH:23]=[N:22][C:13]2=[CH:14][C:15]=1[O:16][C@@H:17]1[CH2:21][O:20][CH2:19][CH2:18]1)=[O:8])[CH3:3].[C:35]([O-:47])(=[O:46])[CH2:36][C:37]([CH2:42][C:43]([O-:45])=[O:44])([C:39]([O-:41])=[O:40])[OH:38]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 311Citric AcidHCID 10184653Afatinib

생성물 1

HCID 86710845HCID 86710845, 화합물수율 57.8%

시약·촉매·용매 1

HCID 702Ethanol용매3회

실험 절차

Ethanol (2 ml) was added to 100 mg (0.205 mmol) afatinib free base and the light yellow solution was stirred at room temperature. A solution of 39.4 mg (0.205 mmol) citric acid in 0.5 ml ethanol was added over the course of 2 min. Another 0.5 ml ethanol was added. Precipitation was observed and the mixture was stirred for 15 min. The solid was filtered, washed with 0.5 ml ethanol and dried on rotary evaporator at 50° C. for 2 h to give 80 mg (57%) of a light yellow solid.

후처리

  1. customPrecipitation
  2. stirringthe mixture was stirred for 15 min
  3. filtrationThe solid was filtered
  4. washwashed with 0.5 ml ethanol
  5. customdried on rotary evaporator at 50° C. for 2 h

출처 및 근거

ORD 기록
ord-951dc02bc7024171a7e52e9c01243158
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09012464B2

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