Methanol → 2-chloro-N-[2-[[(3-chlorophenyl)-methyl]-amino]-ethyl]-9-cyclopentyl-9H-purin-6-amine

HRID 1244944노트

반응식

HRID 1244944 반응식
[NH2:1][CH2:2][CH2:3][NH:4][C:5]1[N:13]=[C:12]([Cl:14])[N:11]=[C:10]2[C:6]=1[N:7]=[CH:8][N:9]2[CH:15]1[CH2:19][CH2:18][CH2:17][CH2:16]1.CO.[Cl:22][C:23]1[CH:24]=[C:25]([CH:28]=[CH:29][CH:30]=1)[CH:26]=O.[BH3-]C#N.[Na+]>C(O)(=O)C>[Cl:14][C:12]1[N:11]=[C:10]2[C:6]([N:7]=[CH:8][N:9]2[CH:15]2[CH2:19][CH2:18][CH2:17][CH2:16]2)=[C:5]([NH:4][CH2:3][CH2:2][NH:1][CH2:26][C:25]2[CH:28]=[CH:29][CH:30]=[C:23]([Cl:22])[CH:24]=2)[N:13]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 114773-ChlorobenzaldehydeHCID 5003444Sodium cyanoborohydrideHCID 21922924N-(2-aminoethyl)-2-chloro-9-cyclopentyl-9H-purin-6-amine

생성물 1

HCID 219229532-chloro-N-[2-[[(3-chlorophenyl)-methyl]-amino]-ethyl]-9-cyclopentyl-9H-purin-6-amine

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

281 mg of the product obtained in Stage 1 of Example 7, 4 ml of methanol, 0.2 ml of 3-chloro-benzaldehyde and 0.2 ml of acetic acid are mixed together, the reaction medium is agitated for 2 hours and 30 minutes, 0.1 g of NaBH3CN is added and agitation is carried out at ambient temperature for 1 hour. After evaporating the solvent, the residue is chromatographed on silica eluting with CH2Cl2/methanol/ammonium hydroxide (95/0.5/0.33) and 172 mg of expected product is obtained.

후처리

  1. waitagitation is carried out at ambient temperature for 1 hour
  2. customAfter evaporating the solvent
  3. customthe residue is chromatographed on silica eluting with CH2Cl2/methanol/ammonium hydroxide (95/0.5/0.33)

출처 및 근거

ORD 기록
ord-d00d1b05e78c414e906892329b3a5628
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07122669B1

반응 노트

불러오는 중…