Diisopropylethylamine → HCID 66940566, 화합물

HRID 1845081노트

반응식

HRID 1845081 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[CH:9]=[N:8][C:7]([C:15]([OH:17])=O)=[CH:6]2.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.[CH2:51]([O:53][C:54]([C:56]1[C:64]2[N:63]=[C:62]([NH2:65])[NH:61][C:60]=2[CH:59]=[C:58]([O:66][CH2:67][CH3:68])[CH:57]=1)=[O:55])[CH3:52]>CN(C=O)C.[Cl-].[Na+].O>[CH2:51]([O:53][C:54]([C:56]1[C:64]2[N:63]=[C:62]([NH:65][C:15]([C:7]3[N:8]=[CH:9][C:10]4[C:5]([CH:6]=3)=[CH:4][C:3]([O:2][CH3:1])=[C:12]([O:13][CH3:14])[CH:11]=4)=[O:17])[NH:61][C:60]=2[CH:59]=[C:58]([O:66][CH2:67][CH3:68])[CH:57]=1)=[O:55])[CH3:52]

참가 물질

7

반응물 4

HCID 81531DiisopropylethylamineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 14278968HCID 14278968, 화합물HCID 66940226HCID 66940226, 화합물

생성물 1

HCID 66940566HCID 66940566, 화합물수율 63%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 57417360Sodium chloride; water용매

실험 절차

235 mg (1.0 mmol) of 6,7-dimethoxy-isoquinoline-3-carboxylic acid and 400 mg (1.0 mmol) of HBTU were dissolved in 1.5 mL of DMF and 0.5 mL of DIEA and treated with 249 mg (1.0 mmol) of 2-amino-6-ethoxy-1H-benzoimidazole-4-carboxylic acid ethyl ester (prepared in Example 471) as described in general procedure A. Upon completion, the reaction was diluted with brine. The resulting solid was filtered, washed with water and EtOAc, and dried under vacuum to produce 290 mg (0.63 mmol, 63%) of 2-[(6,7-dimethoxy-isoquinoline-3-carbonyl)-amino]-6-ethoxy-1H-benzoimidazole-4-carboxylic acid ethyl ester. LCMS: 465 (M+1)+.

후처리

  1. filtrationThe resulting solid was filtered
  2. washwashed with water and EtOAc
  3. customdried under vacuum

출처 및 근거

ORD 기록
ord-5135f67f110945cfb0881ffad5978059
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946259B2

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