Pivaloyl chloride → HCID 54435396, 화합물

HRID 965551노트

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HRID 965551 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]2[C:19]3[C:14](=[CH:15][C:16]([Cl:20])=[CH:17][CH:18]=3)[C:13]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=3[Cl:35])([NH:21][C:22]([N:24]([CH2:27][CH3:28])[CH2:25][CH3:26])=[O:23])[C:12]2=[O:36])(=[O:10])=[O:9])=[CH:4][CH:3]=1.[C:37](Cl)(=[O:42])[C:38]([CH3:41])([CH3:40])[CH3:39]>N1C=CC=CC=1>[C:38]([C:37]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]2[C:19]3[C:14](=[CH:15][C:16]([Cl:20])=[CH:17][CH:18]=3)[C:13]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=3[Cl:35])([NH:21][C:22]([N:24]([CH2:25][CH3:26])[CH2:27][CH3:28])=[O:23])[C:12]2=[O:36])(=[O:10])=[O:9])=[CH:4][CH:3]=1)=[O:42])([CH3:41])([CH3:40])[CH3:39]

참가 물질

4

반응물 2

HCID 62493Pivaloyl chlorideHCID 19076557HCID 19076557, 화합물

생성물 1

HCID 54435396HCID 54435396, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A solution of 0.400 g of the compound obtained in EXAMPLE 13 in 3 ml of pyridine is cooled to 0° C. and 0.100 g of pivaloyl chloride is added. The mixture is stirred for 18 hours, the temperature being allowed to rise to RT, and then evaporated under vacuum. The residue is extracted with AcOEt, washed with a 5% solution of potassium hydrogensulfate, dried over sodium sulfate and evaporated under vacuum. The residue is chromatographed on silica using a DCM/AcOEt mixture (95/5; v/v) as the eluent to give the expected product after crystallization from a DCM/iso ether mixture. m=0.180 g. M.p.=228° C.

후처리

  1. customto rise to RT
  2. customevaporated under vacuum
  3. extractionThe residue is extracted with AcOEt
  4. washwashed with a 5% solution of potassium hydrogensulfate
  5. dry with materialdried over sodium sulfate
  6. customevaporated under vacuum
  7. customThe residue is chromatographed on silica using a DCM/AcOEt mixture (95/5; v/v) as the eluent

출처 및 근거

ORD 기록
ord-ac3206e525544889ba0961844106e1e8
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05773612

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