1,2-Dichloroethane → HCID 11465756, 화합물

HRID 730961노트

반응식

HRID 730961 반응식
[CH3:1][C:2]([CH3:32])([CH3:31])[C:3](=[O:30])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]([C:17]2[CH:18]=[CH:19][C:20]3[CH:24]=[C:23]([C:25](O)=[O:26])[S:22][C:21]=3[CH:28]=2)([CH2:15][CH3:16])[CH2:13][CH3:14])=[CH:8][C:7]=1[CH3:29].C(Cl)CCl.Cl.[CH3:38][NH:39][CH3:40]>C(Cl)Cl.CN(C1C=CN=CC=1)C>[CH3:38][N:39]([CH3:40])[C:25]([C:23]1[S:22][C:21]2[CH:28]=[C:17]([C:12]([C:9]3[CH:10]=[CH:11][C:6]([O:5][CH2:4][C:3](=[O:30])[C:2]([CH3:32])([CH3:31])[CH3:1])=[C:7]([CH3:29])[CH:8]=3)([CH2:15][CH3:16])[CH2:13][CH3:14])[CH:18]=[CH:19][C:20]=2[CH:24]=1)=[O:26]

참가 물질

6

반응물 3

HCID 111,2-DichloroethaneHCID 10473Dimethylamine, hydrochlorideHCID 114651606-{1-[4-(3,3-Dimethyl-2-oxo-butoxy)-3-methyl-phenyl]-1-ethyl-propyl}-benzo[b]thiophene-2-carboxylic acid

생성물 1

HCID 11465756HCID 11465756, 화합물수율 91%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

6-{1-[4-(3,3-Dimethyl-2-oxo-butoxy)-3-methyl-phenyl]-1-ethyl-propyl}-benzo[b]thiophene-2-carboxylic acid (290 mg, 0.642 mmol) in CH2Cl2 (5.0 mL) is treated with DMAP (235 mg, 1.93 mmol) and EDC (184 mg, 0.962 mmol). The mixture is stirred for 15 min at RT, and dimethylamine hydrochloride (78 mg, 0.962 mmol) is added. The reaction is stirred for 18 h and quenched with aqueous NH4Cl (5.0 mL). The organic layer is loaded onto a silica gel column and purified with 50% EtOAc/Hex to afford the title compound (280 mg, 91%).

후처리

  1. stirringThe reaction is stirred for 18 h
  2. customquenched with aqueous NH4Cl (5.0 mL)
  3. custompurified with 50% EtOAc/Hex

출처 및 근거

ORD 기록
ord-1242d6e85e38489bbf26b443ce640d27
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07582775B2

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