Methanol → 4-(9-Thia-1,5,7-triaza-fluoren-8-yl)-piperazine-1-carbothioic acid (benzo[1,3]dioxol-5-ylmethyl)-amide

HRID 1038965

반응식

HRID 1038965 반응식
[N:1]1([C:7]2[C:8]3[S:15][C:14]4[N:16]=[CH:17][CH:18]=[CH:19][C:13]=4[C:9]=3[N:10]=[CH:11][N:12]=2)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.N1C=CC=CC=1.[Cl-].[O:27]1[C:31]2[CH:32]=[CH:33][C:34]([CH2:36][NH:37][CH:38]=[S:39])=[CH:35][C:30]=2[O:29][CH2:28]1.CO>ClCCl>[O:27]1[C:31]2[CH:32]=[CH:33][C:34]([CH2:36][NH:37][C:38]([N:4]3[CH2:3][CH2:2][N:1]([C:7]4[N:12]=[CH:11][N:10]=[C:9]5[C:8]=4[S:15][C:14]4[N:16]=[CH:17][CH:18]=[CH:19][C:13]5=4)[CH2:6][CH2:5]3)=[S:39])=[CH:35][C:30]=2[O:29][CH2:28]1

참가 물질

6

반응물 4

HCID 887MethanolHCID 1049PyridineHCID 673902864-Piperazinopyrido[3',2';4,5]thieno[3,2-d]pyrimidineHCID 86601006N-Benzo[1,3]dioxol-5-ylmethyl-thioformamide chloride

생성물 1

HCID 114198954-(9-Thia-1,5,7-triaza-fluoren-8-yl)-piperazine-1-carbothioic acid (benzo[1,3]dioxol-5-ylmethyl)-amide

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 4-piperazinopyrido[3′,2′;4,5]thieno[3,2-d]pyrimidine (200 mg, 0.74 mmol) and pyridine (0.5 mL, 7.9 mmol) in dichloromethane (20 mL) was added a solution of product 1c in dichloromethane (20 mL) and this was stirred overnight. Methanol was added to quench excess thiophosgene, and the residue after removal of solvent was purified by silica gel column chromatography eluting with 5% methanol/dichloromethane and further recrystallized from dichloromethane/hexane to give 110 mg (32%).

후처리

  1. customto quench excess thiophosgene
  2. customthe residue after removal of solvent
  3. customwas purified by silica gel column chromatography
  4. washeluting with 5% methanol/dichloromethane
  5. customfurther recrystallized from dichloromethane/hexane
  6. customto give 110 mg (32%)

출처 및 근거

ORD 기록
ord-ae3609dde43c4916994449b2a23d5b25
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08552018B2

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