Triethylamine → HCID 86628294, 화합물

HRID 21263노트

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HRID 21263 반응식
[OH:1][C:2]1[C:10]([CH:11]=[O:12])=[CH:9][C:8]([I:13])=[C:7]2[C:3]=1[CH:4]([O:24][CH3:25])[N:5]([C:15]([CH3:23])([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[CH3:16])[C:6]2=[O:14].C(N(CC)CC)C.[CH3:33][S:34](Cl)(=[O:36])=[O:35]>ClCCl>[CH3:33][S:34]([O:1][C:2]1[C:10]([CH:11]=[O:12])=[CH:9][C:8]([I:13])=[C:7]2[C:3]=1[CH:4]([O:24][CH3:25])[N:5]([C:15]([CH3:16])([C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1)[CH3:23])[C:6]2=[O:14])(=[O:36])=[O:35]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 86628295HCID 86628295, 화합물

생성물 1

HCID 86628294HCID 86628294, 화합물수율 100%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In a similar manner to Step 1 of Example 289, 4-hydroxy-5-formyl-3-methoxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone (325 mg, 0.720 mmol) was dissolved in dichloromethane (10 mL), and the solution was treated with triethylamine (0.401 mL, 2.88 mmol) and methanesulfonyl chloride (0.111 mL, 1.43 mmol), followed by purification by flash column chromatography (hexane/ethyl acetate=95/5 to 80/20) to obtain 4-methanesulfonyloxy-5-formyl-3-methoxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone (381 mg, yield 58%).

후처리

  1. customfollowed by purification by flash column chromatography (hexane/ethyl acetate=95/5 to 80/20)

출처 및 근거

ORD 기록
ord-423e7883fbb949c69ff1129c763d1319
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745641B2

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