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Hydrochloric Acid → HCID 69744946, 화합물

HRID 1063914
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HRID 1063914 반응식
C(OC([N:8]1[CH2:14][CH2:13][C@:12]([CH2:29][C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])([C:15]2[S:16][C:17]([C:20]3[CH:25]=[CH:24][C:23]([CH2:26][CH2:27][CH3:28])=[CH:22][CH:21]=3)=[CH:18][CH:19]=2)[S:11](=[O:38])(=[O:37])[CH2:10][CH2:9]1)=O)(C)(C)C.Cl.C(=O)(O)[O-].[Na+]>O1CCCC1>[CH2:26]([C:23]1[CH:22]=[CH:21][C:20]([C:17]2[S:16][C:15]([C@:12]3([CH2:29][C:30]([O:32][C:33]([CH3:34])([CH3:36])[CH3:35])=[O:31])[S:11](=[O:38])(=[O:37])[CH2:10][CH2:9][NH:8][CH2:14][CH2:13]3)=[CH:19][CH:18]=2)=[CH:25][CH:24]=1)[CH2:27][CH3:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 69744461HCID 69744461, 화합물

생성물 1

HCID 69744946HCID 69744946, 화합물수율 104.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of t-butyl 2-[(S)-4-t-butoxycarbonyl-7-(5-(4-propylphenyl)-2-thienyl)-1,1-dioxoperhydro-1,4-thiazepin-7-yl]acetate (10.4 g) in tetrahydrofuran (120 ml) was added conc. hydrochloric acid (30 ml) in tetrahydrofuran (30 ml) under ice-water cooling and the mixture was stirred at ambient temperature for 15 hours. The mixture was basified with saturated sodium bicarbonate solution and extracted with ethyl acetate. The organic layer was separated, washed with brine, dried over magnesium sulfate, and evaporated in vacuo to give t-butyl 2-[(S)-7-(5-(4-propylphenyl)-2-thienyl)-1,1-dioxoperhydro-1,4-thiazepin-7-yl]acetate (8.94 g) as yellow oil.

후처리

  1. extractionextracted with ethyl acetate
  2. customThe organic layer was separated
  3. washwashed with brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-355296f64b574e6893d359cc3443568d
출처 데이터셋
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06967197B2

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