Pivaloyl chloride → 2,4,4'-Tripivaloyloxybenzophenone

HRID 2119170노트

반응식

HRID 2119170 반응식
[OH:1][C:2]1[CH:16]=[C:15]([OH:17])[CH:14]=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1)=[O:5].[C:18](Cl)(=[O:23])[C:19]([CH3:22])([CH3:21])[CH3:20]>N1C=CC=CC=1>[C:18]([O:1][C:2]1[CH:16]=[C:15]([O:17][C:18](=[O:23])[C:19]([CH3:22])([CH3:21])[CH3:20])[CH:14]=[CH:13][C:3]=1[C:4]([C:6]1[CH:7]=[CH:8][C:9]([O:12][C:18](=[O:23])[C:19]([CH3:22])([CH3:21])[CH3:20])=[CH:10][CH:11]=1)=[O:5])(=[O:23])[C:19]([CH3:22])([CH3:21])[CH3:20]

참가 물질

4

반응물 2

HCID 62493Pivaloyl chlorideHCID 738522,4,4'-Trihydroxybenzophenone

생성물 1

HCID 140104022,4,4'-Tripivaloyloxybenzophenone

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A solution of 2.3 g (0.01 mole) of 2,4,4'trihydroxybenzophenone was warmed to 50° C. with 3.65 g (0.035 mole) of pivaloyl chloride in 75 mls of dry pyridine. After 2 hrs. at 5° C., the solvent was evaporated under N2 stream and H2O added to the residue. The oily material was extracted with CH2Cl2 and washed with dilute K2CO3. The organic layer was dried over MgSO4. The glass which was recovered after solvent removal was crystallized from ethanol; 4.20 g (86%) yield; M.P.~94°-96° C.

후처리

  1. customat 5° C., the solvent was evaporated under N2 stream and H2O
  2. additionadded to the residue
  3. extractionThe oily material was extracted with CH2Cl2
  4. washwashed with dilute K2CO3
  5. dry with materialThe organic layer was dried over MgSO4
  6. customThe glass which was recovered
  7. customafter solvent removal
  8. customwas crystallized from ethanol
  9. custom4.20 g (86%) yield

출처 및 근거

ORD 기록
ord-6e738dac7e324a4f9001c1f968844b2c
출처 데이터셋
uspto-grants-1987_07
특허 번호
US04683241

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