Triethylamine → HCID 86628294、化合物

HRID 21263ノート

反応式

HRID 21263 の反応式
[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]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 86628295HCID 86628295、化合物

生成物 1

HCID 86628294HCID 86628294、化合物収率 100%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-423e7883fbb949c69ff1129c763d1319
出典データセット
uspto-grants-2010_06
特許番号
US07745641B2

反応ノート

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