Diethyl Ether → ASTA-Z-7654(free acid)

HRID 1731962노트

반응식

HRID 1731962 반응식
[Cl:1][CH2:2][CH2:3][N:4]([CH2:14][CH2:15][Cl:16])[P:5]1(=[O:13])[NH:10][CH:9](OC)[CH2:8][CH2:7][O:6]1.[CH:17]1([NH3+:23])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1.[SH:24][CH2:25][CH2:26][S:27]([O-:30])(=[O:29])=[O:28].ClC(Cl)(Cl)C(O)=O.CCOCC>CN(C)C=O>[CH:17]1([NH3+:23])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1.[Cl:1][CH2:2][CH2:3][N:4]([CH2:14][CH2:15][Cl:16])[P:5]1(=[O:13])[NH:10][CH:9]([S:24][CH2:25][CH2:26][S:27]([O-:30])(=[O:29])=[O:28])[CH2:8][CH2:7][O:6]1

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 6421Trichloroacetic AcidHCID 230498732-Sulfanylethane-1-sulfonic acid--cyclohexanamine (1/1)HCID 230498792-(bis-(2-chloroethyl)-amino)-4-methoxy-tetrahydro-2H-1,3,2-oxazaphosphorin-2-oxide

생성물 1

HCID 6917796ASTA-Z-7654(free acid)

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2.9 g (10 mmol) of 2-(bis-(2-chloroethyl)-amino)-4-methoxy-tetrahydro-2H-1,3,2-oxazaphosphorin-2-oxide and 2.4 g (10 mmol) of cyclohexylammonium-2-mercaptoethanesulphonate were dissolved with some trichloroacetic acid in 10 ml of dimethylformamide and were stored at -25° C. for 20 hours. After leaving the mixture to stand for another three hours at 0° C., it was mixed with ether until clouding commenced, triturated, the crystallised material was filtered with suction after standing for 20 hours at 0° C., and was washed and dried.

후처리

  1. customAfter leaving the mixture
  2. waitto stand for another three hours at 0° C.
  3. customtriturated
  4. filtrationthe crystallised material was filtered with suction
  5. waitafter standing for 20 hours at 0° C.
  6. washwas washed
  7. customdried

출처 및 근거

ORD 기록
ord-3ca5ca98e1404661871237c0ae6e7762
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04623742

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