Triethylamine → N-[2-[[5-{2,8-Dimethyl-5H-dibenzo[a,d]cyclohepten-5-yl}-3,4-dihydro-2-oxo4-thioxo-1(2H)-pyrimidinyl]methyl]thiazol-4-ylcarbonyl]-L-aspartic acid, dimethyl ester

HRID 1275888

반응식

HRID 1275888 반응식
[CH3:1][C:2]1[CH:34]=[CH:33][C:5]2[CH:6]([C:16]3[C:17](=[S:32])[NH:18][C:19](=[O:31])[N:20]([CH2:22][C:23]4[S:24][CH:25]=[C:26]([C:28]([OH:30])=O)[N:27]=4)[CH:21]=3)[C:7]3[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][C:8]=3[CH:9]=[CH:10][C:4]=2[CH:3]=1.C1N=CN(C(N2C=NC=C2)=O)C=1.[CH3:47][O:48][C:49](=[O:57])[C@H:50]([CH2:52][C:53]([O:55][CH3:56])=[O:54])[NH2:51].C(N(CC)CC)C>CN(C)C=O>[CH3:15][C:12]1[CH:13]=[CH:14][C:7]2[CH:6]([C:16]3[C:17](=[S:32])[NH:18][C:19](=[O:31])[N:20]([CH2:22][C:23]4[S:24][CH:25]=[C:26]([C:28]([NH:51][C@H:50]([C:49]([O:48][CH3:47])=[O:57])[CH2:52][C:53]([O:55][CH3:56])=[O:54])=[O:30])[N:27]=4)[CH:21]=3)[C:5]3[CH:33]=[CH:34][C:2]([CH3:1])=[CH:3][C:4]=3[CH:10]=[CH:9][C:8]=2[CH:11]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 1112071,4-Dimethyl L-aspartateHCID 22117231HCID 22117231, 화합물

생성물 1

HCID 131722226N-[2-[[5-{2,8-Dimethyl-5H-dibenzo[a,d]cyclohepten-5-yl}-3,4-dihydro-2-oxo4-thioxo-1(2H)-pyrimidinyl]methyl]thiazol-4-ylcarbonyl]-L-aspartic acid, dimethyl ester

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

The product from example 8(0.4 g) was dissolved in dry dimethylformamide (15 ml) and treated with N,N-carbonyldiimidazole (0.16 g). After 30 minutes L-aspartic acid dimethyl ester (0.32 g) was added followed by triethylamine (0.5 ml). The mixture was stirred overnight and partitioned between ethyl acetate and 2M HCl. The organic phase was washed with brine, dried (MgSO4), evaporated and purified by chromatography eluting with 50% ethyl acetate in dichloromethane. Used directly in the next step.

후처리

  1. custompartitioned between ethyl acetate and 2M HCl
  2. washThe organic phase was washed with brine
  3. dry with materialdried (MgSO4)
  4. customevaporated
  5. custompurified by chromatography
  6. washeluting with 50% ethyl acetate in dichloromethane

출처 및 근거

ORD 기록
ord-12675a682fa14479ba65271d789b59f9
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06162808

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