Triethylamine → 2-(1-oxido-2,3-dihydro-1,4-benzothiazepin-4(5H)-yl)-6-methylthieno[3,2-d]pyrimidin-4(3H)-one

HRID 1910453노트

반응식

HRID 1910453 반응식
Cl[C:2]1[NH:3][C:4](=[O:12])[C:5]2[S:10][C:9]([CH3:11])=[CH:8][C:6]=2[N:7]=1.[CH:13]1[C:18]2[CH2:19][NH:20][CH2:21][CH2:22][S:23](=[O:24])[C:17]=2[CH:16]=[CH:15][CH:14]=1.C(N(CC)CC)C>C1(C)C=CC=CC=1>[O:24]=[S:23]1[C:17]2[CH:16]=[CH:15][CH:14]=[CH:13][C:18]=2[CH2:19][N:20]([C:2]2[NH:3][C:4](=[O:12])[C:5]3[S:10][C:9]([CH3:11])=[CH:8][C:6]=3[N:7]=2)[CH2:21][CH2:22]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 196082032,3,4,5-Tetrahydrobenzo[f][1,4]thiazepine 1-oxideHCID 1363597872-chloro-6-methylthieno[3,2-d]pyrimidin-4(3H)-one

생성물 1

HCID 1363597882-(1-oxido-2,3-dihydro-1,4-benzothiazepin-4(5H)-yl)-6-methylthieno[3,2-d]pyrimidin-4(3H)-one수율 81.1%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

2-Chloro-6-methylthieno[3,2-d]pyrimidin-4(3H)-one (3.01 g, 15 mmol) was dissolved in toluene (50 mL), followed by addition of 6,7,8,9-tetrahydro-5-thia-8-aza-benzocycloheptene-5-oxide (3.39 g, 18.7 mmol), triethylamine (6 mL, 43 mmol). Then the solution was heated to reflux overnight. The suspension was filtrated and the solid was washed by methanol to afford 4.2 g of 2-(1-oxido-2,3-dihydro-1,4-benzothiazepin-4(5H)-yl)-6-methylthieno[3,2-d]pyrimidin-4(3H)-one (yield was 81.1%) as a slight brown solid. MS obsd. (ESI+) [(M+H)+] 346.

후처리

  1. temperatureThen the solution was heated
  2. temperatureto reflux overnight
  3. filtrationThe suspension was filtrated
  4. washthe solid was washed by methanol

출처 및 근거

ORD 기록
ord-546760932c7d4ce7851aa7b19caadd55
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08604019B2

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