Hydrochloric Acid → HCID 178441229, 화합물

HRID 406281노트

반응식

HRID 406281 반응식
CC([N:5]([C@H:9]1[CH2:12][C@@H:11]([O:13][C:14]2[CH:19]=[C:18]([F:20])[C:17]([C:21]([CH3:24])([CH3:23])[CH3:22])=[C:16]([F:25])[CH:15]=2)[CH2:10]1)C(=O)[O-])(C)C.[ClH:26]>O1CCOCC1>[ClH:26].[CH3:24][C:21]([C:17]1[C:16]([F:25])=[CH:15][C:14]([O:13][C@@H:11]2[CH2:10][C@H:9]([NH2:5])[CH2:12]2)=[CH:19][C:18]=1[F:20])([CH3:22])[CH3:23]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 178441232HCID 178441232, 화합물

생성물 1

HCID 178441229HCID 178441229, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

To a stirred solution of 1,1-dimethylethyl(cis-3-{[4-(1,1-dimethylethyl)-3,5-difluorophenyl]oxy}cyclobutyl)carbamate (6.85 g, 19.27 mmol) in 1,4-dioxane (50 mL) was added a solution of hydrogen chloride in 1,4-dioxane (50 mL, 4M, 200 mmol) in one charge. The reaction vessel was sealed and the reaction stirred at ambient temperature for 16 hours. The reaction was concentrated to approximately half volume in vacuo and the resultant slurry was diluted with diethyl ether (200 mL) and the mixture stirred rapidly for 10 min. The precipitate was collected by filtration and dried in vacuo to give the title compound as a white solid (3.39 g). The mother liquors were concentrated in vacuo to give a yellow sticky solid. Trituration with diethyl ether (ca 20 mL) gave a white precipitate, the precipitate was collected by filtration and dried in vacuo to give a further batch of the title compound (1.035 g).

후처리

  1. additioncharge
  2. customThe reaction vessel was sealed
  3. concentrationThe reaction was concentrated to approximately half volume in vacuo
  4. additionthe resultant slurry was diluted with diethyl ether (200 mL)
  5. stirringthe mixture stirred rapidly for 10 min
  6. filtrationThe precipitate was collected by filtration
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-ca05047150f34cbabfa39b630f1e541c
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08754101B2

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