Trichloroacetic Acid → ASTA-Z-7654(free acid)

HRID 1731963

반응식

HRID 1731963 반응식
[CH2:1]1[CH:7](O)[NH:6][P:4]([N:9]([CH2:13][CH2:14][Cl:15])[CH2:10][CH2:11][Cl:12])(=[O:5])[O:3][CH2:2]1.[CH:16]1([NH3+:22])[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1.[SH:23][CH2:24][CH2:25][S:26]([O-:29])(=[O:28])=[O:27].ClC(Cl)(Cl)C(O)=O>CO>[CH:16]1([NH3+:22])[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1.[Cl:12][CH2:11][CH2:10][N:9]([CH2:13][CH2:14][Cl:15])[P:4]1(=[O:5])[NH:6][CH:7]([S:23][CH2:24][CH2:25][S:26]([O-:29])(=[O:28])=[O:27])[CH2:1][CH2:2][O:3]1

참가 물질

5

반응물 3

HCID 6421Trichloroacetic AcidHCID 997354-HydroxycyclophosphamideHCID 230498732-Sulfanylethane-1-sulfonic acid--cyclohexanamine (1/1)

생성물 1

HCID 6917796ASTA-Z-7654(free acid)

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

1.4 g (5 mmol) of 4-hydroxycyclophosphamide and 1.2 g (5 mmol) of cyclohexylammonium-2-mercaptoethanesulphonate were dissolved together with a trace of trichloroacetic acid in 25 ml of methanol and were left to stand overnight in a refrigerator at -25° C. The reaction solution was then concentrated to about 5 ml, ether was added until clouding commenced and the mixture was triturated. The crystallised material was filtered with suction after standing for 20 hours at 0° C., and was washed and dried.

후처리

  1. waitwere left
  2. concentrationThe reaction solution was then concentrated to about 5 ml, ether
  3. additionwas added
  4. customthe mixture was triturated
  5. filtrationThe crystallised material was filtered with suction
  6. waitafter standing for 20 hours at 0° C.
  7. washwas washed
  8. customdried

출처 및 근거

ORD 기록
ord-78d36a09114c45999debc021d0f1fa0b
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04623742

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