Acetic Acid → HCID 178508982, 화합물

HRID 982495노트

반응식

HRID 982495 반응식
O.[NH2:2][C:3]1[N:8]=[C:7]([OH:9])[CH:6]=[C:5](Cl)[N:4]=1.[S:11]1[CH:15]=[CH:14][CH:13]=[C:12]1[CH2:16][NH2:17].C(N(CC)CC)C.C(O)(=O)C>COC(O)C>[NH2:2][C:3]1[N:8]=[C:7]([OH:9])[CH:6]=[C:5]([NH:17][CH2:16][C:12]2[S:11][CH:15]=[CH:14][CH:13]=2)[N:4]=1

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 8471TriethylamineHCID 34005(2-Thienylmethyl)amineHCID 178508975HCID 178508975, 화합물

생성물 1

HCID 178508982HCID 178508982, 화합물

시약·촉매·용매 1

HCID 30156371-Methoxyethanol용매

실험 절차

2-Amino-6-chloro-4-pyrimidinol, monohydrate (85%, 100 g, 0.5197 mol) was suspended in methoxyethanol (700 ml) and 2-thienylmethylamine (96%, 61.3 g, 0.5197 mol) was added to the suspension. The mixture was heated under reflux for two hours and then 73 ml (d=0.726; 0.52 mol) of triethylamine was added and the refluxing continued for an additional 18 hours. The reaction mixture was poured into ice water (1000 ml), acidified with acetic acid (ph 4.0) and the precipitated solid was filtered, washed, and dried. Yield: 110 g (72.6%). This was used in the next step without further purification.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for two hours
  3. filtrationthe precipitated solid was filtered
  4. washwashed
  5. customdried
  6. customThis was used in the next step without further purification

출처 및 근거

ORD 기록
ord-e93c8902a2ea439498c48473c8816209
출처 데이터셋
uspto-grants-1991_02
특허 번호
US04996319

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