Hydrochloric Acid → HCID 178428844, 화합물

HRID 269420노트

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HRID 269420 반응식
[Cl-].[NH2:2][C:3]([NH2:5])=[NH2+:4].CC([O-])(C)C.[K+].[CH3:12][S:13]([C:16]1[C:17]([O:27][C:28]2[CH:33]=[CH:32][C:31]([S:34]([CH3:37])(=[O:36])=[O:35])=[C:30]([S:38]([F:43])([F:42])([F:41])([F:40])[F:39])[CH:29]=2)=[CH:18][C:19]([CH3:26])=[C:20]([CH:25]=1)[C:21](OC)=[O:22])(=[O:15])=[O:14].Cl>CN(C=O)C.O>[CH3:12][S:13]([C:16]1[C:17]([O:27][C:28]2[CH:33]=[CH:32][C:31]([S:34]([CH3:37])(=[O:35])=[O:36])=[C:30]([S:38]([F:41])([F:43])([F:42])([F:39])[F:40])[CH:29]=2)=[CH:18][C:19]([CH3:26])=[C:20]([CH:25]=1)[C:21]([NH:4][C:3]([NH2:5])=[NH:2])=[O:22])(=[O:14])=[O:15]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 5460839Carbamimidoylazanium ChlorideHCID 23665647Potassium tert-butoxideHCID 59832571Methyl 5-methanesulfonyl-4-(4-methanesulfonyl-3-pentafluorosulfanylphenoxy)-2-methylbenzoate

생성물 1

HCID 178428844HCID 178428844, 화합물수율 79.9%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

546 mg of guanidinium chloride and 535 mg of KOtBu were stirred in 20 ml of anhydrous DMF at RT for 30 minutes. Then 500 mg of methyl 5-methanesulfonyl-4-(4-methanesulfonyl-3-pentafluorosulfanylphenoxy)-2-methylbenzoate were added, and the mixture was left to stand at RT for 16 h. The reaction mixture was poured into 20 ml of water, adjusted to pH=8 with aqueous HCl solution and extracted 3 times with 50 ml of EA each time. The combined EA phases were then washed with 20 ml of a 5% aqueous NaHCO3 solution and dried over MgSO4, and the solvent was removed in vacuo. 420 mg of an amorphous solid were obtained.

후처리

  1. waitthe mixture was left
  2. extractionextracted 3 times with 50 ml of EA each time
  3. washThe combined EA phases were then washed with 20 ml of a 5% aqueous NaHCO3 solution
  4. dry with materialdried over MgSO4
  5. customthe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-adee3046077d45a2809439c3b8fecdbe
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07446225B2

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