HCID 21273587, 화합물 → HCID 178429718, 화합물

HRID 846909노트

반응식

HRID 846909 반응식
[SH:1][C:2]1[N:7]2[N:8]=[C:9]([C:11](OC)=[O:12])[N:10]=[C:6]2[N:5]=[C:4]([CH3:15])[CH:3]=1.[H-].C([Al+]CC(C)C)C(C)C.CCCCCC>O1CCCC1>[SH:1][C:2]1[N:7]2[N:8]=[C:9]([CH2:11][OH:12])[N:10]=[C:6]2[N:5]=[C:4]([CH3:15])[CH:3]=1

참가 물질

4

반응물 2

HCID 21273587HCID 21273587, 화합물HCID 178499048HCID 178499048, 화합물

생성물 1

HCID 178429718HCID 178429718, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

2.24 g of methyl 7-mercapto-5-methyl-s-triazolo[1,5-a]-pyrimidine-2-carboxylate were suspended in 350 ml of tetrahydrofuran and treated at 2° within 15 minutes with 40 ml of a 1M diisobutylaluminium hydride/hexane solution. The reaction mixture was stirred at 2° for 10 minutes and subsequently treated with ice. The reaction mixture was concentrated extensively, the residue was taken up in 30 ml of water, and the solution was acidified to pH 1.2 with concentrated hydrochloric acid. The solid was collected by filtration and dried in a high vacuum. There was obtained 7-mercapto-5-methyl-s-tria-zolo[1,5-a]pyrimidine-2-methanol of melting point 233° (dec.).

후처리

  1. additionsubsequently treated with ice
  2. concentrationThe reaction mixture was concentrated extensively
  3. filtrationThe solid was collected by filtration
  4. customdried in a high vacuum

출처 및 근거

ORD 기록
ord-b45379e3a06f4054b076533b8fd9cceb
출처 데이터셋
uspto-grants-1992_08
특허 번호
US05138066

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