Water → 4-(4-tert-Butylbenzoylamino)isophthalic acid

HRID 1247178노트

반응식

HRID 1247178 반응식
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[C:11]([OH:13])=[O:12].O.[C:15]([C:19]1[CH:27]=[CH:26][C:22]([C:23](Cl)=[O:24])=[CH:21][CH:20]=1)([CH3:18])([CH3:17])[CH3:16]>CC(C)=O>[C:15]([C:19]1[CH:20]=[CH:21][C:22]([C:23]([NH:1][C:2]2[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=2[C:11]([OH:13])=[O:12])=[O:24])=[CH:26][CH:27]=1)([CH3:18])([CH3:16])[CH3:17]

참가 물질

5

반응물 3

HCID 962WaterHCID 743724-tert-Butylbenzoyl chlorideHCID 113558524-Aminobenzene-1,3-dioic acid

생성물 1

HCID 219064144-(4-tert-Butylbenzoylamino)isophthalic acid수율 29%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

Into 60 mL acetone was dissolved 0.905 g (5 mmol) 4-aminoisophthalic acid. To the solution was added 30 mL water. The mixture was cooled in an ice bath, and 1.08 mL (5.5 mmol) 4-tert-butylbenzoyl chloride in 10 mL acetone was added dropwise. The mixture was allowed to warm slowlyly to room temperature and after 24 h was concentrated under vacuum and shaken between EtOAc (150 mL) and cold dilute HCl (150 mL). The organic layer was dried (MgSO4) and evaporated. The desired crystalline product (0.489 g, 29%) was obtained from methylene chloride-hexane.

후처리

  1. temperatureThe mixture was cooled in an ice bath
  2. concentrationwas concentrated under vacuum
  3. dry with materialThe organic layer was dried (MgSO4)
  4. customevaporated

출처 및 근거

ORD 기록
ord-9ca1d60fb6c443faac0c4569fa720387
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07129245B2

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